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CuNCs熒光探針檢測環(huán)境水樣中的孔雀石綠

劉梅¹，林洪¹，吳云英¹，胡棟寶¹，伍賢學(xué)¹，余琴¹，陳文靜^*1，謝建新^*2

（1. 玉溪師范學(xué)院化學(xué)生物與環(huán)境學(xué)院，玉溪 653100；2. 黔南民族師范學(xué)院化學(xué)化工學(xué)院，都勻 55800）

摘要：以Cu（NO₃）₂為原料，D-青霉胺（DPA）為還原劑和穩(wěn)定劑，采用一鍋法在室溫下制備出高量子產(chǎn)率的紅色熒光銅納米簇（CuNCs），構(gòu)建了一種可簡單快速檢測孔雀石綠（MG）的熒光探針。優(yōu)化了CuNCs的合成條件，采用透射電子顯微鏡（TEM）、X射線光電子能譜（XPS）、傅里葉變換紅外光譜（FT-IR）對(duì)CuNCs的形貌及組成進(jìn)行了表征。MG對(duì)CuNCs具有選擇性猝滅效應(yīng)，在1~75 μmol/L濃度范圍內(nèi)，MG的濃度與CuNCs的熒光強(qiáng)度（F₀/F）呈良好的線性關(guān)系，檢出限為0.75 μmol/L。該熒光探針成功用于湖水中MG的靈敏檢測，加標(biāo)回收率為99.1%~109.9%。該方法可用于環(huán)境水樣中MG的高靈敏檢測。

關(guān)鍵詞：銅納米簇；孔雀石綠；熒光猝滅

中圖分類號(hào)：O657.3    文獻(xiàn)標(biāo)識(shí)碼：A    文章編號(hào)：1000-0720（2023）10-1279-06

CuNCs fluorescent probe for the detection of malachite green in environmental water samples

LIU Mei¹，LIN Hong¹，WU Yunying¹，HU Dongbao¹，WU Xianxue¹，YU Qin¹，CHEN Wenjing^*1，XIE Jianxin^*2

1. School of Chemistry，Biology and Environment，Yuxi Normal University，Yuxi 653100，China；2. School of Chemistry and Chemical Engineering，Qiannan Normal University for Nationalites，Duyun 55800，China）

Abstract：Using copper nitrate as raw material and D-penicillamine （DPA） as reducing and stabilizing agent，red fluorescent copper nanoclusters （CuNCs） with high quantum yield were prepared by one-pot method at room temperature，and then a fluorescent probe for simple and rapid detection of malachite green （MG） was established. The synthesis conditions were optimized，and the morphology and composition of CuNCs were characterized by transmission electron microscope （TEM），X-ray photoelectron spectroscopy （XPS） and Fourier transform infrared spectrometer （FT-IR）. The fluorescence of CuNCs could be selectively quenched by MG. The fluorescence intensity of CuNCs （F₀/F） had a good linear relationship with the concentration of MG in the range of 1-75 μmol/L，and the detection limit was as low as 0.75 μmol/L. The fluorescence probe was successfully used for the sensitive detection of MG in lake water，and the recoveries were 99.1%-109.9%. The proposed method could be applied for highly sensitive detection of MG in environmental water samples.

Keywords：copper nanoclusters （CuNCs）；malachite green （MG）；fluorescence quenching 

微型近紅外光譜法快速檢測賽買提杏糖度

彭娟¹，邵學(xué)廣^*2，楚剛輝^*1

（1. 新疆特色藥食用植物資源化學(xué)實(shí)驗(yàn)室，喀什大學(xué)化學(xué)與環(huán)境科學(xué)學(xué)院，喀什 844000；2. 南開大學(xué)化學(xué)學(xué)院分析科學(xué)研究中心，天津 300071）

摘要：為實(shí)現(xiàn)賽買提杏糖度（SSC）的快速檢測，并建立一個(gè)穩(wěn)健的預(yù)測模型，本文使用微型近紅外光譜儀采集光譜，數(shù)顯糖度計(jì)測定SSC，對(duì)比了連續(xù)小波變換（CWT）、卷積平滑（SG）、多元散射校正（MSC）、標(biāo)準(zhǔn)正態(tài)變換（SNV）、一階導(dǎo)（1^st），二階導(dǎo)（2^nd）及其兩兩組合的光譜預(yù)處理方法建模結(jié)果，結(jié)果顯示，CWT，CWT+MSC和CWT+SNV 3種方法結(jié)果較好。以這3種預(yù)處理方法為基礎(chǔ)，對(duì)比了競爭自適應(yīng)加權(quán)抽樣（CARS）、隨機(jī)化試驗(yàn)（RT）、蒙特卡羅-無信息變量消除法（MC-UVE）和C值法4種變量選擇方法，分別得出與杏糖度相關(guān)的光譜變量，建立了賽買提杏糖度偏最小二乘（PLS）預(yù)測模型，經(jīng)CWT+MSC光譜預(yù)處理加C值法變量選擇建立的PLS模型最佳，其預(yù)測相關(guān)系數(shù)（R_p）從0.844優(yōu)化到0.960，預(yù)測均方根誤差（RMSEP）從1.273降低到0.699，相對(duì)分析偏差（RPD）從1.853上升到3.430。結(jié)果表明，適當(dāng)光譜預(yù)處理和變量選擇能有效提高賽買提杏糖度快速無損檢測的效率和準(zhǔn)確性。

關(guān)鍵詞：賽買提杏；變量選擇；近紅外光譜；糖度

中圖分類號(hào)：O657.3    文獻(xiàn)標(biāo)識(shí)碼：A    文章編號(hào)：1000-0720（2023）10-1285-07

Rapid detection of Cymaiti apricot soluble 

solids content by miniature near infrared spectroscopy

PENG Juan¹，SHAO Xueguang^*2，CHU Ganghui^*1

1. Chemistry Laboratory of Xinjiang Special Medicinal Edible Plant Resources，College of Chemistry and Environmental Science，Kashi University，Kashi 844000，China；2. Analytical Science Research Center，School of Chemistry，Nankai University，Tianjin 300071，China）

Abstract：To realize the rapid detection of Cymaiti apricot soluble solids content （SSC） and establish a steady prediction model of SSC，a miniature near-infrared spectrometer was used to collect the spectra，and a digital display sugar meter was used to determine the SSC.Then the modeling results including continuous wavelet transform（CWT），Savitzky-Golay（SG smoothing），multiplicative scatter correction（MSC），standard normal variate（SNV），firstderivative（1^st），second derivative（2^nd） and the spectral pretreatment method of two combinations were compared，and the models of CWT，CWT+MSC and CWT+SNV showed good results. Based on above three pretreatment methods，four variable selection methods including competitive adaptive reweighted sampling （CARS），randomization test （RT），informative variables elimination （MC-UVE） and C value were compared by obtaining the spectral variables related to SSC of apricot. And the partial least squares （PLS） prediction model of apricot SSC was established. The best model was established by CWT+MSC peretreatment combined with C value variable selection method. The correlation coefficient （R_p） of prediction set increased from 0.844 to 0.960，the root mean square error of prediction （RMSEP） set decreased from 1.273 to 0.699，and the relative percent deviation （RPD） increased from 1.853 to 3.430.The results showed that spectral pretreatement and variable selection properly could effectively improve the efficiency and accuracy of the portable and rapid nondestructive testing of apricot SSC.

Keywords：Cymaiti apricot；variable selection；near infrared spectroscopy；soluble solids content （SSC）

破乳誘導(dǎo)萃取食用植物油中營養(yǎng)元素的原子發(fā)射光譜分析

李愛陽¹，陳宇¹，殷子懿¹，黃建華^*2

（1. 湖南工學(xué)院化學(xué)與環(huán)境工程學(xué)院，衡陽 421002；2. 湖南省中醫(yī)藥研究院中藥研究所，長沙 410013）

摘要：基于破乳誘導(dǎo)萃取，提出利用微波等離子體原子發(fā)射光譜（MP-AES）測定食用植物油中多種營養(yǎng)元素的新策略。采用5%（w/V）的Triton X‐114為乳化劑，50%（V/V）的HCl為萃取劑，對(duì)食用植物油樣品于90 ℃下超聲水浴40 min，將分析元素從有機(jī)基質(zhì)轉(zhuǎn)移至酸性水相，采用MP-AES測定其中的8種營養(yǎng)元素（K，Na，Ca，Mg，F(xiàn)e，Mn，Cu，Zn）。8種元素在各自質(zhì)量濃度范圍內(nèi)呈良好的線性關(guān)系，線性相關(guān)系數(shù)（R）≥0.9998，檢出限（LOD）在0.16~1.95 μg/L之間，樣品的加標(biāo)回收率在94.0%~105.0%之間，相對(duì)標(biāo)準(zhǔn)偏差（RSD）≤4.0%。本方法測定結(jié)果與國標(biāo)法基本一致。應(yīng)用所建立的方法對(duì)市場上不同產(chǎn)地的花生油、玉米油、油菜籽油、山茶油、葵花籽油和橄欖油進(jìn)行檢測，6種食用植物油中富含8種營養(yǎng)元素。本方法已用于食用植物油中營養(yǎng)元素的質(zhì)量評(píng)價(jià)。

關(guān)鍵詞：破乳誘導(dǎo)萃取；食用植物油；微波等離子體原子發(fā)射光譜；營養(yǎng)元素

中圖分類號(hào)：O657.31    文獻(xiàn)標(biāo)識(shí)碼：A    文章編號(hào)：1000-0720（2023）10-1292-07

Determination of nutrient elements in edible vegetable oil 

by atomic emission spectroscopy based on extraction induced by emulsion breaking

LI Aiyang¹，CHEN Yu¹，YIN Ziyi¹，HUANG Jianhua^*2

1. Department of Chemical and Environmental Engineering，Hunan Institute of Technology，Hengyang 421002，China；2. Institute of Chinese Materia，Hunan Academy of Traditional Chinese Medicine，Changsha 410013，China）

Abstract：A new strategy for the determination of multiple nutrient elements in edible vegetable oil using microwave plasma atomic emission spectroscopy （MP-AES） was proposed based on the extraction induced by emulsion breaking. Using 5% （w/V） Triton X-114 as emulsifier and 50% （V/V） hydrochloric acid as extractant，the edible vegetable oil samples were subjected to ultrasonic water bath at 90 ℃ for 40 min，leading to the analytes transferred from organic matrix to acidic aqueous phase. The eight kinds of nutrient elements （K，Na，Ca，Mg，F(xiàn)e，Mn，Cu and Zn） were determined by MP-AES. The linear correlation coefficients of the analytes in their respective mass concentration ranges were no less than 0.9998，showing good linear relationships. The limits of detection （LODs） were 0.16-1.95 μg/L，and the spiked recoveries were 94.0%-105.0%，with the relative standard deviations （RSDs） no higher than 4.0%. The results of this method were basically consistent with that of the standard method. The developed method was used to detect nutrient elements in peanut oil，corn oil，rapeseed oil，camellia oil，sunflower oil and olive oil from different origins in the domestic market. The results showed 6 kinds of edible vegetable oils were rich in 8 kinds of nutrient elements. The method has been used for the quality evaluation of nutrient elements in edible vegetable oil.

Keywords：extraction induced by emulsion breaking；edible vegetable oil；microwave plasma atomic emission spectroscopy；nutrient elements

復(fù)合納米酶傳感器可視化檢測水中汞離子

趙鳳霞^1，2，李丹靚^1，2，陳果¹，邵飛¹，劉思汝¹，嚴(yán)杭麗^1，2，鄭毅^1，2，楊勝園^*1，2，梁好^*1，2

（1. 南華大學(xué)衡陽醫(yī)學(xué)院，衡陽 421001；2. 衡陽市健康危害因子檢驗(yàn)檢疫新技術(shù)研究重點(diǎn)實(shí)驗(yàn)室，衡陽 421001）

摘要：基于貴金屬銀修飾的單壁碳納米管（Ag-SWNTs）復(fù)合納米酶的催化作用及L-半胱氨酸（L-Cys）和汞離子（Hg²⁺）的特異性結(jié)合作用，建立了一種快速檢測Hg²⁺的可視化比色方法。在適宜的pH條件下，當(dāng)Hg²⁺不存在時(shí)，L-Cys可抑制Ag-SWNTs酶活性，使得3，3’，5，5’-四甲基聯(lián)苯胺（TMB）無法被催化氧化顯色；而當(dāng)Hg²⁺存在時(shí)，Hg²⁺可特異性結(jié)合L-Cys，Ag-SWNTs的酶活性不被抑制，TMB被催化氧化為oxTMB，溶液顏色發(fā)生由無色至藍(lán)色的變化。在最佳實(shí)驗(yàn)條件下，該檢測體系在最大吸收波長653 nm處的吸光度值與1.35~90.91 μg/mL范圍內(nèi)的Hg²⁺濃度呈良好的線性關(guān)系，回歸方程為ΔA=0.0076c-0.085，相關(guān)系數(shù)是0.9930，檢出限為0.44 μg/mL。該方法應(yīng)用于環(huán)境水中Hg²⁺的測定，加標(biāo)回收率為92.4%~99.9%。

關(guān)鍵詞：單壁碳納米管；L-半胱氨酸；汞離子檢測；納米酶；催化作用

中圖分類號(hào)：R115    文獻(xiàn)標(biāo)識(shí)碼：A    文章編號(hào)：1000-0720（2023）10-1299-05

Visual detection of mercury ions based on composite nano-enzyme sensor

ZHAO Fengxia^1，2，LI Danliang^1，2，CHEN Guo¹，SHAO Fei¹，LIU Siru¹，YAN Hangli^1，2，ZHENG Yi^1，2，YANG Shengyuan^*1，2，LIANG Hao^*1，2

1. Hengyang Medical School，University of South China，Hengyang 421001，China；2. Key Laboratory of Hengyang for Health Hazard Factors Inspection and Quarantine，Hengyang 421001，China）

Abstract：A new colorimetric method was established for the rapid visual detection of Hg²⁺ based on the catalysis of silver modified single wall carbon nanotubes （Ag-SWNTs） and the specific binding of L-Cys and mercury ions （Hg²⁺）. In the absence of Hg²⁺ at appropriate pH，L-gystein （L-Cys） can inhibit the enzymatic activity of Ag-SWNTs to catalyze the chromogenic reaction of 3，3'，5，5'-tetramethylbenzidine （TMB）. while in the presence of Hg²⁺，Hg²⁺ can specifically bind to L-Cys to keep the enzymatic activity of Ag-SWNTs，TMB was catalyzed and oxidized to oxTMB，and the color of the solution changed from colorless to blue. Under the optimal experimental conditions，the absorbance value of the detection system at the maximum absorption wavelength of 653 nm had a good linear relationship with the concentration of Hg²⁺ in the range of 1.35-90.91 μg/mL，and the linear regression equation was ΔA=0.0076c-0.085，with the relative correlation coefficient （r） of 0.9930. The limit of detection （LOD） for Hg²⁺ was 0.44 μg/mL. This method can be applied to determine Hg²⁺ in environmental water，and the recoveries for spiking experiments were 92.4%-99.9%.

Keywords：single-walled carbon nanotube；L-cysteine；the detection of mercury ions；nano-enzyme；catalytic action

超聲法制備環(huán)糊精-鉑納米酶并用于檢測葡萄糖

姜翠鳳^*1，2，王金山¹，阮志凡¹，熊芳芳¹，劉星宇¹，劉藝媛¹，郭偉¹

（1. 鹽城工學(xué)院材料科學(xué)與工程學(xué)院，鹽城 224051；2. 鹽城工學(xué)院江蘇省生態(tài)環(huán)境材料重點(diǎn)實(shí)驗(yàn)室，鹽城 224051）

摘要：通過超聲輔助法制備了具有類過氧化物酶、類氧化物酶和類過氧化氫酶活性的β-環(huán)糊精-鉑納米粒子（CD-PtNPs），該納米材料在同一酸度條件下同時(shí)具有3種類酶活性。對(duì)影響其類過氧化物酶活性的因素進(jìn)行了優(yōu)化，最佳條件為：溫度20 ℃，pH 3.6，3，3’，5，5’-四甲基聯(lián)苯胺（TMB）濃度2 mmol/L，H₂O₂ 濃度78 μmol/L，CD-PtNPs用量0.648 μg。基于其類過氧化物酶活性，構(gòu)建了可通過比色和紫外可見吸收光譜檢測葡萄糖的傳感平臺(tái)。該傳感平臺(tái)在緩沖溶液中對(duì)葡萄糖的檢出限為80 μmol/L，在30%（V/V）血清中檢出限為0.18 mmol/L。CD-PtNPs制備方法簡便、快速且可避免聚集，有望在生物分析領(lǐng)域得到廣泛應(yīng)用。

關(guān)鍵詞：超聲輔助合成；納米酶；鉑納米材料；葡萄糖；傳感器

中圖分類號(hào)：O657.31；X832    文獻(xiàn)標(biāo)識(shí)碼：A    文章編號(hào)：1000-0720（2023）10-1304-07

Ultrasound-assisted synthesis of 

β-cyclodextrin-platinum nanozyme and its application for glucose detection

JIANG Cuifeng^*1，2，WANG Jinshan¹，RUAN Zhifan¹，XIONG Fangfang¹，LIU Xingyu¹，LIU Yiyuan¹，GUO Wei¹

1. School of Materials Science and Engineering，Yancheng Institute of Technology，Yancheng 224051，China；2. Key Laboratory for Ecological-Environment Materials of Jiangsu Province，Yancheng Institute of Technology，Yancheng 224051，China）

Abstract：β-cyclodextrin-platinum nanoparticles （CD-PtNPs） with peroxidase-，oxidase- and catalase-like activity were prepared by an ultrasound-assisted reduction method. The optimal conditions for peroxidase-like activity were as follows：20 ℃，pH 3.6，2 mmol/L of TMB，78 μmol/L of H₂O₂ and 0.648 μg of CD-PtNPs. Based on the excellent peroxidase-like activity，the limit of detection （LOD） for glucose was of 80 μmol/L. Furthermore，this method allowed rapid detection of glucose in 30% （V/V） serum with LOD of 0.18 mmol/L. This ultrasound-assisted method could be expanded to prepare other kind of nanozymes，and CD-PtNPs were expected to have wide application in bioanalytical chemistry.

Keywords：ultrasound-assisted synthesis；nanozyme；Pt nanoparticles；glucose；sensor

一種基于香豆素的熒光探針的合成及其對(duì)鋁離子和鋅離子的識(shí)別

李娜，李政^*，王樹軍，陳鈺，肖立偉

（廊坊師范學(xué)院化學(xué)與材料科學(xué)學(xué)院，廊坊 065000）

摘要：設(shè)計(jì)合成了以4-甲基-7-羥基-8-醛基香豆素為熒光團(tuán)，4-氨基安替比林為識(shí)別位點(diǎn)的探針ACAP，通過紅外光譜、核磁共振氫譜及碳譜對(duì)探針的結(jié)構(gòu)進(jìn)行了表征。利用熒光光譜研究了探針對(duì)不同金屬離子的識(shí)別性能。結(jié)果顯示，在CH₃OH/Tris-HCl（9∶1，V∶V）緩沖溶液中，探針ACAP對(duì)Al³⁺和Zn²⁺具有選擇性識(shí)別及良好的識(shí)別靈敏性。離子競爭實(shí)驗(yàn)顯示，其它共存離子對(duì)探針識(shí)別Al³⁺/Zn²⁺幾乎沒有影響，表明探針具有良好的抗干擾性。結(jié)合比測試顯示，探針ACAP與Al³⁺和Zn²⁺均以1∶1結(jié)合。探針ACAP對(duì)Al³⁺和Zn²⁺的檢出限分別為1.78 μmol/L和0.194 μmol/L，均低于世衛(wèi)組織（WHO）對(duì)飲用水中Al³⁺和Zn²⁺所允許的最高濃度。

關(guān)鍵詞：香豆素；鋁離子；鋅離子；熒光探針；性能

中圖分類號(hào)：O657.31；X832    文獻(xiàn)標(biāo)識(shí)碼：A    文章編號(hào)：1000-0720（2023）10-1311-06

Synthesis and properties of a coumarin-based

 fluorescent probe for the detection of Al³⁺ and Zn²⁺

LI Na，LI Zheng^*，WANG Shujun，CHEN Yu，XIAO Liwei

College of Chemistry and Materials Science，Langfang Normal University，Langfang 065000，China）

Abstract：A probe ACAP was designed and synthesized using 4-methyl-7-hydroxy-8-uronic coumarin as fluorophore and 4-amino-antipyrine as recognition site. The structure of the probe was characterized by infrared spectrum，¹H-NMR and ¹³C-NMR spectra. The recognition performance of the probe for different metal ions was investigated by fluorescence spectroscopy. The results showed that the probe ACAP had a selective recognition and a good sensitivity to Al³⁺ and Zn²⁺ in CH₃OH/Tris-HCl （9∶1，V∶V） buffer solution. Ion competition experiments revealed that other co-existing ions had little effects on Al³⁺/Zn²⁺ recognition，indicating that the probe possessed a good anti-interference. Binding ratio test manifested that the probe ACAP bond with Al³⁺/Zn²⁺ in a 1∶1 manner. The detection limits for Al³⁺ and Zn²⁺ were estimated to be 1.78 μmol/L and 0.194 μmol/L，respectively，which were lower than the permissible concentrations of Al³⁺ and Zn²⁺ described by World Health Organization （WHO） in drinking water.

Keywords：coumarin；Al³⁺；Zn²⁺；fluorescence probe；properties

基于三螺旋適體探針的雙向開關(guān)傳感同時(shí)靈敏測定四環(huán)素和氯霉素

王子棋，高亞芳，譚心韻，李安祺，魯理平^*

（北京工業(yè)大學(xué)環(huán)境科學(xué)系，區(qū)域大氣復(fù)合污染防治北京市重點(diǎn)實(shí)驗(yàn)室，北京100124）

摘要：設(shè)計(jì)了基于發(fā)卡狀三螺旋結(jié)構(gòu)的DNA分子開關(guān)熒光傳感器，利用適配體特異性識(shí)別，實(shí)現(xiàn)了對(duì)2種目標(biāo)抗生素的同時(shí)靈敏測定。其分子開關(guān)結(jié)構(gòu)由一個(gè)特異性適配體識(shí)別序列和一個(gè)雙標(biāo)記的信號(hào)探針序（STP）列組成發(fā)卡狀三螺旋結(jié)構(gòu)。識(shí)別四環(huán)素的STP兩端用芘分子修飾，識(shí)別氯霉素的信號(hào)探針兩端分別用硫化鎘量子點(diǎn)（CdS QDs）和金納米粒子（AuNPs）修飾，適配體序列插入環(huán)狀（Loop）區(qū)域形成三鏈結(jié)構(gòu)。目標(biāo)抗生素存在時(shí)，識(shí)別探針與之結(jié)合，釋放出信號(hào)探針，致使兩端發(fā)光物質(zhì)靠近，熒光信號(hào)發(fā)生顯著變化。傳感器的熒光發(fā)光強(qiáng)度與四環(huán)素和氯霉素濃度呈良好的線性關(guān)系，線性范圍為1×10^-3~10 μmol/L，檢出限為0.3 nmol/L。該方法用于測定雞蛋中的四環(huán)素和氯霉素，結(jié)果滿意。

關(guān)鍵詞：四環(huán)素；氯霉素；三螺旋DNA；分子開關(guān)；熒光傳感器

中圖分類號(hào)：O657.3    文獻(xiàn)標(biāo)識(shí)碼：A    文章編號(hào)：1000-0720（2023）10-1317-07

Simultaneous and sensitive determination of tetracycline 

and chloramphenicol by two-way switch sensing based on triple helix aptamer probe

WANG Ziqi，GAO Yafang，TAN Xinyun，LI Anqi，LU Liping^*

Key Laboratory of Beijing on Regional Air Pollution Control，F(xiàn)aculty of Environment Science，Beijing University of Technology，Beijing 100124，China）

Abstract：A DNA molecular switch fluorescence sensor based on hairpin triple helix structure was designed to achieve simultaneous sensitive determination of two target antibiotics by aptamer specific recognition. The molecular switching structure consists of a specific aptamer recognition sequence and a double-labeled signal probe sequence. The two ends of the signal probe for tetracycline recognition were modified with pyrene molecules，and the two ends of the signal probe for chloramphenicol recognition were modified with cadmium sulfide quantum dots （CdS QDs） and gold nanoparticles，respectively. The aptamer sequence was inserted into the loop region to form a three-chain structure. When the target antibiotic was present，the recognition probe bound to it and released a signal probe，bringing the luminescent substance at both ends closer together，and the fluorescence signal changed significantly （enhanced or reduced）. The fluorescence intensity of the sensor showed a good linear relationship with the concentrations of tetracycline and chloramphenicol，the linear range was 1×10^-3-10 μmol/L，and the detection limit was 0.3 nmol/L. The method was used to determine tetracycline and chloramphenicol in eggs with satisfactory results.

Keywords：tetracycline；chloromycetin；triple-helix DNA；molecular switch；fluorescence sensor

毛細(xì)管內(nèi)標(biāo)定量核磁共振波譜法測定滴眼液中氧氟沙星含量

曾貝怡¹，史丹陽¹，劉兆鑫¹，郭強(qiáng)勝¹，李靜²，許旭^*1

（1. 上海應(yīng)用技術(shù)大學(xué)化學(xué)與環(huán)境工程學(xué)院，上海 201418；2. 上海通微分析技術(shù)有限公司，上海 201203）

摘要：建立了一種毛細(xì)管內(nèi)標(biāo)封管的定量核磁共振波譜（qNMR）法測定滴眼液中氧氟沙星的含量。將內(nèi)標(biāo)物鄰苯二甲酸氫鉀溶于氘代試劑重水并預(yù)先封入毛細(xì)管中，分別用已知含量的3種純品測定其校正因子（k）為0.03125±0.00033，該值穩(wěn)定且與樣品無關(guān)，可直接用于測定其他成分。將其用于測定滴眼液樣品中氧氟沙星的含量，以δ 1.53 ppm （H-14，d，J=6.5 Hz，3H）為定量峰。實(shí)驗(yàn)結(jié)果表明，氧氟沙星濃度和氧氟沙星與內(nèi)標(biāo)定量峰面積比值呈線性關(guān)系，線性相關(guān)系數(shù)為0.9999，檢出限為0.03 mg/mL。方法日內(nèi)相對(duì)標(biāo)準(zhǔn)偏差（RSD）為0.5%，加標(biāo)回收率為98.8%~103.9%。本方法操作簡便、結(jié)果準(zhǔn)確，減少了內(nèi)標(biāo)與氘代試劑的用量。

關(guān)鍵詞：定量核磁共振波譜法；毛細(xì)管內(nèi)標(biāo)；氧氟沙星；滴眼液

中圖分類號(hào)：O657.2    文獻(xiàn)標(biāo)識(shí)碼：A    文章編號(hào)：1000-0720（2023）10-1324-08

Determination of ofloxacin in eye drops by quantitative 

nuclear magnetic resonance spectroscopy using capillary internal standard

ZENG Beiyi¹，SHI Danyang¹，LIU Zhaoxin¹，GUO Qiangsheng¹，LI Jing²，XU Xu^*1

1. School of Chemical and Environmental Engineering，Shanghai Institute of Technology，Shanghai 201418，China；2. Unimicro （Shanghai） Technologies Co.，Ltd.，Shanghai 201203，China）

Abstract：A quantitative nuclear magnetic resonance spectroscopy （qNMR） method using capillary internal standard was presented and applied for the determination of ofloxacin in eye drops. The internal standard of potassium hydrogen phthalate was dissolved in deuterium reagent and pre-sealed into a capillary. The internal standard capillary was placed into a nuclear magnetic tube containing the sample and used for qNMR determination. The correction factor （k） of an internal standard capillary was detected as 0.03125±0.00033 using 3 kinds of pure compounds with known contents. The k value was stable and independent of the sample，and could be applied for the direct determination of other components. For the qNMR determination of ofloxacin content in eye drops，the peak at δ 1.53 ppm （H-14，d，J=6.5 Hz，3H） was selected as the quantitative peak. The results showed that the correlation coefficient was 0.9999 for the linear curve between ofloxacin concentration and the peak area ratio of ofloxacin to internal standard，and the limit of detection （LOD） was 0.03 mg/mL. The relative standard deviation （RSD） of the method was 0.5%，and the recoveries were 98.8%-103.9%. The qNMR method using internal standard sealed capillary tube was simple and accurate，and decreased the consumption of internal standard and deuterium reagents.

Keywords：quantitative nuclear magnetic resonance spectroscopy；capillary internal standard；ofloxacin；eye drops

兩階段相關(guān)系數(shù)波長選擇方法

萬巖¹，陳爭光^*1，焦峰²

（1. 黑龍江八一農(nóng)墾大學(xué)信息與電氣工程學(xué)院，大慶 163319；2. 黑龍江八一農(nóng)墾大學(xué)農(nóng)學(xué)院，大慶 163319）

摘要：為降低建立模型的復(fù)雜度，提高近紅外光譜模型的預(yù)測精度，提出一種兩階段相關(guān)系數(shù)（TSCC）波長選擇方法。先計(jì)算各波長點(diǎn)向量和濃度向量之間的相關(guān)系數(shù)，選擇相關(guān)系數(shù)較大的波長點(diǎn)作為第一階段波長。在此基礎(chǔ)上計(jì)算各個(gè)波長點(diǎn)之間的相關(guān)系數(shù)，選擇與其他波長點(diǎn)之間相關(guān)系數(shù)較小的波長作為建模波長。采用2組公開數(shù)據(jù)集對(duì)算法進(jìn)行驗(yàn)證，在第一階段波長選擇結(jié)果和兩階段波長選擇結(jié)果上分別建立偏最小二乘回歸（PLSR）模型和多元線性回歸（MLR）模型。結(jié)果表明，基于TSCC波長選擇算法建立的MLR模型（TSCC-MLR），性能優(yōu)于基于全譜的PLSR模型（Full-PLSR）、優(yōu)于基于第一階段波長選擇結(jié)果建立的PLSR模型（CC-PLSR）和基于連續(xù)投影算法（SPA）選擇的數(shù)據(jù)建立的MLR模型（SPA-MLR）。玉米數(shù)據(jù)SPA-MLR模型決定系數(shù)R²為0.8353，CC-PLSR模型R²為0.8652，TSCC-MLR模型R²為0.8951。土壤樣本的近紅外光譜數(shù)據(jù)集，基于TSCC算法提取變量后，得到18個(gè)特征波長并建立MLR模型，R²達(dá)到0.9688，相較于CC-PLSR和SPA-MLR模型，模型預(yù)測性能有所提升。通過2個(gè)數(shù)據(jù)集得到的結(jié)果，證明了本文所提出的TSCC波長選擇方法是一種有效的變量選擇方法。

關(guān)鍵詞：近紅外光譜；特征波長選擇；相關(guān)系數(shù)；多元線性回歸

中圖分類號(hào)：O657.33；S132    文獻(xiàn)標(biāo)識(shí)碼：A    文章編號(hào)：1000-0720（2023）10-1332-09

A wavelength selection method based on two-stage correlation coefficient

WAN Yan¹，CHEN Zhengguang^*1，JIAO Feng²

1. College of Electrical and Information，Heilongjiang Bayi Agricultural University，Daqing 163319，China；2. Agriculture College，Heilongjiang Bayi Agricultural University，Daqing 163319，China）

Abstract：To simplify model construction and increase the precision of near-infrared spectrum （NIRS） prediction models，a two-stage correlation coefficient （TSCC） wavelength selection method was proposed. The correlation coefficient between each wavelength vector and the concentration vector was first calculated，and the wavelength with the larger correlation coefficient was chosen as the result of the first stage wavelength selection. Based on this，the correlation coefficient between each wavelength was calculated，and the modeling wavelength was chosen based on the wavelength with the lowest correlation coefficient to the other wavelengths. The algorithm was validated using two publicly accessible datasets，and models for partial least squares regression （PLSR） and multiple linear regression （MLR） were created on the outcomes of the first stage wavelength selection and the second stage wavelength selection，respectively. According to the findings，the PLSR model based on the outcomes of the first stage wavelength selection （CC-PLSR），the PLSR model based on full spectra （Full-PLSR），and the MLR model based on data selected by the successive projections algorithm （SPA） （SPA-MLR） were all underperformed by the TSCC-MLR，which was the MLR model based on the wavelength selected by TSCC. Based on the corn dataset，the coefficient of determination （R²） of SPA-MLR，CC-PLSR and TSCC-MLR model were 0.8353，0.8652 and 0.8951，respectively. The NIR spectra of soil samples were extracted by TSCC technology to acquire 18 distinctive wavelengths. The MLR model was developed based on these wavelengths，R_p² of 0.9688. Compared with the CC-PLSR model and SPA-MLR model，the prediction performance of MLR model was enhanced. The results of two datasets showed that the two-stage correlation coefficient wavelength selection method proposed in this paper was an effective variable selection method.

Keywords：near infrared spectroscopy；characteristic wavelength selection；correlation coefficient；multiple linear regression

高效液相色譜法測定化妝品中禁用芳香胺1-萘胺和2-萘胺及其鹽類

孟憲雙¹，牛增元²，羅忻²，劉藝靜^1，3，白樺¹，馬強(qiáng)^*1

（1. 中國檢驗(yàn)檢疫科學(xué)研究院，北京 100176；2. 青島海關(guān)技術(shù)中心，青島 266109；3. 北京中醫(yī)藥大學(xué)中藥學(xué)院，北京 102488）

摘要：建立了化妝品中禁用芳香胺1-萘胺和2-萘胺同分異構(gòu)體及其鹽類的高效液相色譜分析方法。膏霜和乳液類試樣依次經(jīng)氯化鈉破乳、溶劑萃取；水劑類試樣直接經(jīng)超聲輔助溶劑萃取。萃取液經(jīng)Waters Sep-Pak C₁₈固相萃取柱凈化后由XBridge BEH Phenyl色譜柱分離，以0.02 mol/L磷酸二氫鈉溶液和甲醇為流動(dòng)相梯度洗脫，二極管陣列檢測器測定，檢測波長240 nm，外標(biāo)法定量。在優(yōu)化的樣品前處理和色譜條件下，1-萘胺和2-萘胺實(shí)現(xiàn)基線分離，檢出限和定量限分別為0.5 μg/kg和1.0 μg/kg，平均回收率為88.7%~107.3%，相對(duì)標(biāo)準(zhǔn)偏差為2.3%~6.8%。該方法解決了法規(guī)明確而技術(shù)空白的問題，適用于化妝品的日常檢驗(yàn)及質(zhì)量控制。

關(guān)鍵詞：固相萃取；高效液相色譜法；禁用芳香胺；同分異構(gòu)體；化妝品

中圖分類號(hào)：O657.7    文獻(xiàn)標(biāo)識(shí)碼：A    文章編號(hào)：1000-0720（2023）10-1341-06

Determination of prohibited aromatic amines of 1-naphthylamine

 and 2-naphthylamine and their salts in cosmetics by high-performance liquid chromatography

MENG Xianshuang¹，NIU Zengyuan²，LUO Xin²，LIU Yijing^1，3，BAI Hua¹，MA Qiang^*1

1. Chinese Academy of Inspection and Quarantine，Beijing 100176，China；2.Technology Center of Qingdao Customs，Qingdao 266109，China；3. School of Chinese Materia Medica，Beijing University of Chinese Medicine，Beijing 102488，China）

Abstract：A high-performance liquid chromatography （HPLC） method was established for the analysis of the prohibited aromatic amines of 1-naphthylamine and 2-naphthylamine isomers and their salts in cosmetics. The cream and emulsion samples were successively demulsified by sodium chloride and extracted by solvent，while the lotion samples were directly subjected to ultrasound-assisted solvent extraction. And the extracts were purified by a Waters Sep-Pak C₁₈ solid-phase extraction column and separated by an XBridge BEH Phenyl chromatographic column，along with gradient elution using 0.02 mol/L sodium dihydrogen phosphate solution and methanol as mobile phase at detection wavelength of 240 nm with diode array detector，and quantified by external standard method. Under the optimized pretreatment and chromatographic conditions，1-naphthylamine and 2-naphthylamine were baseline separated. The limits of detection and limits of quantitation were 0.5 and 1.0 μg/kg，respectively. The average recoveries were 88.7%-107.3%，and the relative standard deviations were 2.3%-6.8%. The method could solve the problem of clear regulations but technical blank，and is suitable for daily inspection and quality control of cosmetics.

Keywords：solid-phase extraction；high-performance liquid chromatography；prohibited aromatic amines；isomers；cosmetics

天冬氨酸修飾納米金-紙芯片體系對(duì)高半胱氨酸的選擇性檢測

張劍^1，2，鄭志鴻¹，張丹¹，張博^1，2，李文靜^1，2，李一冰¹，夏敏珠¹，劉春葉^*1，2

（1. 西安醫(yī)學(xué)院藥學(xué)院，西安 710021；2. 西安醫(yī)學(xué)院藥物研究所，西安 710021）

摘要：建立了以紙芯片為分析平臺(tái)的高半胱氨酸（Hcy）快速檢測新方法。Hcy使天冬氨酸（Asp）修飾的納米金（Asp-AuNPs）體系發(fā)生團(tuán)聚，溶液由紅色逐漸變?yōu)樗{(lán)色。使用手機(jī)拍照記錄結(jié)果，Photoshop軟件分析顯色強(qiáng)度。紅/藍(lán)通道顏色比值（ΔRed/Blue）與Hcy濃度在0.74~74 μmol/L范圍內(nèi)呈良好線性關(guān)系，回歸方程為y=0.0704x+0.5445，相關(guān)系數(shù)（R）為0.9995，檢出限為0.37 μmol/L，加標(biāo)回收率為98.7%~100.3%。共存還原性物質(zhì)干擾誤差在±2%以內(nèi)。該方法測得人血漿中Hcy含量為（5.52±0.39） μmol/L，符合人體血漿中Hcy濃度參考范圍。

關(guān)鍵詞：納米金；微流控紙基分析平臺(tái)；高半胱氨酸；比色法

中圖分類號(hào)：O652    文獻(xiàn)標(biāo)識(shí)碼：A    文章編號(hào)：1000-0720（2023）10-1347-04

Selective determination of homocysteine by a paper-based 

assay system using aspartic acid modified gold nanoparticles

ZHANG Jian^1，2，ZHENG Zhihong¹，ZHANG Dan¹，ZHANG Bo^1，2，LI Wenjing^1，2，LI Yibing¹，XIA Minzhu¹，LIU Chunye^*1，2

1. School of Pharmacy，Xi'an Medical University，Xi'an 710021，China；2. Institute of Medicine，Xi'an Medical University，Xi'an 710021，China）

Abstract：A novel method for homocysteine （Hcy） determination on paper-based analytical devices using aspartic acid （Asp） modified gold nanoparticles （Asp-AuNPs） was proposed. Hcy interacts with Asp-AuNPs selectively and leads to the aggregation of Asp-AuNPs after its addition. A color change from red to blue can be observed on the paper-based analytical devices. The results were recorded using a common cell phone and subsequently analyzed by Photoshop software. The ratio of color intensity at red and blue channel （ΔRed/Blue） increased linearly in the Hcy concentration range of 0.74-74 μmol/L，with the relative coefficient （R） of 0.9995. The regression equation was y=0.0704x+0.5445，the limit of detection was 0.37 μmol/L，and the recoveries of this method were 98.7%-100.3%. The interference deviations of coexisting reductive substances to Hcy were in the range of -2% to 2%. The Hcy concentration in human plasma was determined as （5.52±0.39） μmol/L by this method，which was consistent with the reference range of Hcy.

Keywords：gold nanoparticles；micro?uidic paper-based analytical devices；homocysteine；colorimetric assay

低共熔溶劑液液微萃取-高效液相色譜法測定奶茶中3種甲基黃嘌呤類物質(zhì)

張悅，楊楠，趙思睿，徐凡，謝哲浩，劉彥^*

（河北醫(yī)科大學(xué)藥學(xué)院，石家莊 050017）

摘要：建立了基于低共熔溶劑（DES）的液液微萃取-高效液相色譜法（HPLC）測定奶茶中可可堿、咖啡因和茶堿含量的方法。制備了8種不同組成的DES，并選擇百里酚-辛酸摩爾比為2∶1的DES為萃取溶劑。在優(yōu)化的樣品前處理及色譜條件下，可可堿、咖啡因和茶堿分別在0.1~50.0 μg/mL濃度范圍內(nèi)線性關(guān)系良好，相關(guān)系數(shù)（r）分別為0.9981，0.9988和0.9975，檢出限（LOD）分別為0.06，0.05，0.06 μg/mL，加標(biāo)回收率為93.8%~102.7%，相對(duì)標(biāo)準(zhǔn)偏差（RSD）≤3.9%。該方法適用于測定奶茶中可可堿、咖啡因和茶堿的含量。

關(guān)鍵詞：低共熔溶劑；甲基黃嘌呤類；奶茶；液液微萃取；樣品前處理

中圖分類號(hào)：X132    文獻(xiàn)標(biāo)識(shí)碼：A    文章編號(hào)：1000-0720（2023）10-1351-06

Deep eutectic solvent based liquid liquid microextraction-high performance 

liquid chromatography for the determination of three kinds of methylxanthines in milky tea

ZHANG Yue，YANG Nan，ZHAO Sirui，XU Fan，XIE Zhehao，LIU Yan^*

School of Pharmacy，Hebei Medical University，Shijiazhuang 050017，China）

Abstract：A method of liquid-liquid microextraction （LLME） based on deep eutectic solvent （DES） combined with high performance liquid chromatography （HPLC） was established to detect the contents of theophylline，theobromine and caffeine in milky tea. 8 kinds of DESs with different composition were prepared，and DES with the molar ratio of 5-methyl-2-isopropylphenol to octanoic acid of 2∶1 was selected as the extraction solvent. Under the optimized conditions，there were good linear relationships of theophylline，theobromine and caffeine in the range of 0.1-50.0 μg/mL，with the correlation coefficients （r） of 0.9981，0.9988 and 0.9975，respectively. The limits of detection （LODs） of theophylline，theobromine and caffeine were 0.06，0.05 and 0.06 μg/mL，and the average recoveries were 93.8%-102.7%，respectively. With the relative standard deviations （RSDs） less than 3.9%. This method can be applied to detect the contents of three kinds of methylxanthines in milky tea.

Keywords：deep eutectic solvent；methylxanthines；milky tea；liquid-liquid microextraction；sample pretreatment

氣相色譜-質(zhì)譜法測定廢液樣品中化武相關(guān)化合物

吳姬娜，劉石磊，李曉森，閆瓏，邢中方，楊旸^*

（國民核生化災(zāi)害防護(hù)國家重點(diǎn)實(shí)驗(yàn)室，北京 102205）

摘要：國際禁化武組織（OPCW）每年定期對(duì)各締約國實(shí)驗(yàn)室進(jìn)行分析能力驗(yàn)證，確保指定實(shí)驗(yàn)室能夠勝任真實(shí)樣品分析任務(wù)。2021年第50次水平考試由OPCW中心實(shí)驗(yàn)室進(jìn)行配樣，共配制6個(gè)廢液樣品。采用氣相色譜-質(zhì)譜法對(duì)6個(gè)考試廢液樣品進(jìn)行分析鑒定，最終檢出7個(gè)化武相關(guān)化合物。通過液液萃取、改變色譜固定相選擇性等方法，實(shí)現(xiàn)了目標(biāo)物與背景干擾的有效分離；結(jié)合電子轟擊電離、化學(xué)電離、串聯(lián)質(zhì)譜分析等方式，完成了目標(biāo)化合物結(jié)構(gòu)的準(zhǔn)確鑒定，所得結(jié)果與考試后OPCW發(fā)布的添加化合物清單一致。在鑒定的化合物中有2個(gè)為新型化武相關(guān)化合物，對(duì)其進(jìn)行了質(zhì)譜碎裂分析，為相關(guān)化學(xué)戰(zhàn)劑降解、洗消的后續(xù)研究提供參考。

關(guān)鍵詞：化武相關(guān)化合物；能力驗(yàn)證；廢液樣品；氣相色譜-質(zhì)譜法

中圖分類號(hào)：O657.63    文獻(xiàn)標(biāo)識(shí)碼：A    文章編號(hào)：1000-0720（2023）10-1357-07

Determination of chemical weapons convention-related compounds 

in waste samples by gas chromatography-mass spectrometry

WU Jina，LIU Shilei，LI Xiaosen，YAN Long，XING Zhongfang，YANG Yang^*

State Key Laboratory of NBC Protection for Civilian，Beijing 102205，China）

Abstract：Organization for the Prohibition of Chemical Weapons （OPCW） conducts the official proficiency tests annually among Member States’ laboratories to ensure that the designated laboratories maintain the technical competence for the analysis of authentic samples. Six waste samples were prepared by the OPCW Laboratory for the 50^th proficiency test in 2021. In this paper，all the six waste samples were analyzed by gas chromatography-mass spectrometry，and seven compounds related to the Chemical Weapons Convention were detected. The target chemicals were effectively separated from the background substances by liquid-liquid extraction or column phase selectivity by different stationary phase selection. The structures of the seven compounds were unambiguously identified by the combination of electron ionization，chemical ionization and tandem mass spectrometry modes，and the results were consistent with the spiking chemical list released by OPCW after the test. Among the identified chemicals，there are two novel Chemical Weapon Convention-related chemicals. The fragmentation pathways were presented in details，which may provide useful reference for the subsequent investigation on degradation and decontamination of the related chemical warfare agents.

Keywords：chemical weapons convention-related compounds；proficiency test；waste sample；gas chromatography-mass spectrometry

哌嗪類新精神活性物質(zhì)BZP及TFMPP拉曼光譜特性研究

吳國萍^*1，2，胡辰辰^1，2，陸騰³，吳元釗⁴

（1. 江蘇警官學(xué)院刑事科學(xué)技術(shù)系，南京 210031；2. 江蘇省食品藥品與環(huán)境犯罪檢驗(yàn)技術(shù)工程研究中心，南京 210031；3. 中國科學(xué)院計(jì)算機(jī)網(wǎng)絡(luò)信息中心高性能計(jì)算技術(shù)與應(yīng)用發(fā)展部，北京100083；4. 浙江警察學(xué)院刑事科學(xué)技術(shù)系，浙江省毒品防控技術(shù)研究重點(diǎn)實(shí)驗(yàn)室，杭州 310051）

摘要：運(yùn)用密度泛函理論（DFT）優(yōu)化哌嗪類新精神活性物質(zhì)1-芐基哌嗪（BZP）和1-（3-三氟甲基苯基）哌嗪（TFMPP）的幾何構(gòu)型，結(jié)合實(shí)驗(yàn)測得的拉曼譜圖對(duì)標(biāo)準(zhǔn)品拉曼譜圖的振動(dòng)模式進(jìn)行指認(rèn)和歸屬，并與低濃度樣品的表面增強(qiáng)拉曼（SERS）譜圖進(jìn)行比較；使用自制納米金、NaCl溶液為助劑，優(yōu)化BZP和TFMPP的SERS檢測條件。在最優(yōu)條件下，BZP和TFMPP的檢出限分別為10 ng/mL和1 μg/mL；重復(fù)性實(shí)驗(yàn)中2種樣品的主要特征峰強(qiáng)度相對(duì)標(biāo)準(zhǔn)偏差（RSD）分別4.5%~14%和4.0%~16%。運(yùn)用基于Matlab自行開發(fā)的設(shè)計(jì)分子光譜數(shù)據(jù)分析系統(tǒng)的BP神經(jīng)網(wǎng)絡(luò)模塊，對(duì)模擬未知樣品進(jìn)行預(yù)測，30份BZP樣品和26份TFMPP樣品的預(yù)測值與真實(shí)值比值的平均值（AVG）分別為1.21和0.99，RSD分別為22%和14%。本文可為BZP和TFMPP的拉曼檢測提供理論依據(jù)和快檢方法。

關(guān)鍵詞：密度泛函理論；表面增強(qiáng)拉曼光譜；BP神經(jīng)網(wǎng)絡(luò)；哌嗪類新精神活性物質(zhì)

中圖分類號(hào)：O657.37    文獻(xiàn)標(biāo)識(shí)碼：A    文章編號(hào)：1000-0720（2023）10-1364-09

Study of surface enhanced Raman spectroscopy

 of 1-benzylpiperazine and 1-（3-trifluoromethyl phenyl） piperazine

WU Guoping^*1，2，HU Chenchen^1，2，LU Teng³，WU Yuanzhao⁴

1. Department of Criminal Science and Technology，Jiangsu Police Institute，Nanjing 210031，China；2. Jiangsu Provincial Engineering Research Center for Technical and Criminal Inspection of Food，Drug and Environmental Cases，Nanjing 210031，China；3. Department of High Performance Computing Technology and Application Development，Computer Network Information Center，Chinese Academy of Sciences，Beijing 100083，China；4. Key Laboratory of Drug Prevention and Control Technology of Zhejiang Province，Department of Criminal Science and Technology，Zhejiang Police College，Hangzhou 310051，China）

Abstract：Density functional theory（DFT） was used to optimize and calculate the vibrational wavenumbers of new psychoactive piperazines 1-benzylpiperazine （BZP） and 1-（3-trifluoromethyl phenyl） piperazine （TFMPP），and the samples of BZP and TFMPP were tested by Raman and surface enhanced Raman spectroscopy （SERS）. The Raman spectra of standard samples were compared with the surface enhanced Raman spectra of low concentration. The SERS detection conditions of BZP and TFMPP were optimized by using self-made gold nanoparticles and NaCl solution as additives. Under the optimal detection conditions，the detection limits of BZP and TFMPP were 10 ng/mL and 1 μg/mL，and the relative standard deviations （RSDs） of the main characteristic peak intensities were 4.5%-14% and 4.0%-16%，respectively. BP neural network was used to predict the unknown sample concentration. The average values of the ratio between the predicted value and the true value （AVG） of 30 BZP samples and 26 TFMPP samples were 1.21 and 0.99，with the RSDs of 22% and 14%，respectively. In this paper，the theoretical basis and rapid detection methods for BZP and TFMPP were provided.

Keywords：density functional theory；surface enhanced Raman spectroscopy；BP neural network；new psychoactive piperazines

一測多評(píng)法測定化妝品中的21種防曬劑

王繼雙，李莉^*，王海燕^*

（中國食品藥品檢定研究院，國家藥品監(jiān)督管理局化妝品研究與評(píng)價(jià)重點(diǎn)實(shí)驗(yàn)室，北京 100050）

摘要：基于一測多評(píng)法同時(shí)測定化妝品中21種防曬劑含量。采用高效液相色譜法檢測，以甲醇、四氫呋喃和高氯酸溶液為流動(dòng)相，梯度洗脫，在C₁₈色譜柱上分離21種防曬劑。選取二苯酮-3為內(nèi)部參照物，建立其他20種防曬劑的相對(duì)校正因子，計(jì)算各組分含量。實(shí)驗(yàn)結(jié)果表明，21種防曬劑在一定質(zhì)量濃度范圍內(nèi)線性關(guān)系良好，各組分在24 h內(nèi)穩(wěn)定。一測多評(píng)法和外標(biāo)法測定結(jié)果的相對(duì)平均偏差均不大于4.25%，2種方法結(jié)果的一致性良好。該方法可用于防曬類化妝品防曬劑的測定和質(zhì)量控制。

關(guān)鍵詞：化妝品；防曬劑；一測多評(píng)；高效液相色譜

中圖分類號(hào)：O657.7    文獻(xiàn)標(biāo)識(shí)碼：A    文章編號(hào)：1000-0720（2023）10-1373-07

Analysis of 21 sunscreen agents in cosmetics

with quantitative analysis of multi-components by single marker

WANG Jishuang，LI Li^*，WANG Haiyan^*

National Institutes for Food and Drug Control，Key Laboratory for Researching and Evaluation of Cosmetics of National Medical Products Administration，Beijing 100050，China）

Abstract：A quantitative analysis of multi-components by single marker （QAMS） method for the determination of 21 kinds of sunscreen agents in cosmetics was established. Using methanol，tetrahydrofuran and perchloric acid as mobile phases，21 kinds of sunscreen agents were separated on a C₁₈ column and detected by high performance liquid chromatography （HPLC） with gradient elution. Diphenylketone-3 was selected as the internal reference substance，and the relative correction factors of the other 20 kinds of sunscreen agents were established to calculate the content of each component. The results showed that the 21 kinds of sunscreen agents had good linear relationships within a certain mass concentration ranges，and each component was stable for 24 h. The results of QAMS were close to that of external standard method （ESM），and the relative error was not higher than 4.25%. This method can be used for the determination and quality control of sunscreen agents in cosmetics.

Keywords：cosmetics；sunscreen；quantitative analysis of multi-components by single marker；high performance liquid chromatography

高效鄰苯二甲酸新戊二醇聚酯毛細(xì)管柱的制備及應(yīng)用

石昆，秦金平^*，徐國慶，魏昊東

（南京工業(yè)大學(xué)化工學(xué)院，南京 211816）

摘要：用鄰苯二甲酸和新戊二醇合成了鄰苯二甲酸新戊二醇聚酯，并對(duì)其進(jìn)行了核磁和紅外光譜表征，確定了該物質(zhì)的微觀結(jié)構(gòu)。使用超細(xì)SiO₂載體水溶液對(duì)毛細(xì)管柱內(nèi)壁進(jìn)行表面粗糙化處理，以鄰苯二甲酸新戊二醇聚酯為固定相，配制5 mg/mL的固定液，用靜態(tài)法涂漬了毛細(xì)管色譜柱，制備了0.25 mm×30 m×0.32 μm鄰苯二甲酸新戊二醇聚酯毛細(xì)管柱。以甲酚、二甲酚異構(gòu)體的分離能力評(píng)價(jià)其分離性能。結(jié)果表明，鄰苯二甲酸新戊二醇聚酯毛細(xì)管柱對(duì)甲酚、二甲酚異構(gòu)體具有良好的分離能力，每米理論塔板數(shù)在3000左右，其最高使用溫度為250 ℃。建立了用于檢測高純度間甲酚、對(duì)甲酚的方法。

關(guān)鍵詞：鄰苯二甲酸新戊二醇聚酯；毛細(xì)管色譜；甲酚異構(gòu)體；二甲酚異構(gòu)體

中圖分類號(hào)：O657.7+1    文獻(xiàn)標(biāo)識(shí)碼：A    文章編號(hào)：1000-0720（2023）10-1380-06

Preparation and application of high efficiency

 neopentyl glycol phthalate polyester capillary column

SHI Kun，QIN Jinping^*，XU Guoqing，WEI Haodong

College of Chemical Engineering，Nanjing Technology University，Nanjing 211816，China）

Abstract：Neopentyl glycol phthalate polyester was synthesized from phthalic acid and neopentyl glycol，and its microstructure was characterized by nuclear magnetic resonance （NMR） and infrared radiation （IR）. The inner wall of capillary column was roughened by using ultrafine SiO₂ carrier aqueous solution. The capillary chromatography column （0.25 mm×30 m×0.32 μm） was successfully prepared by static method，using neopentyl glycol phthalate polyester （5 mg/mL） as stationary phase. The separation performance of cresol and xylenol isomers was evaluated. The results showed that the capillary column of neopentyl phthalate had good separation ability for cresol and xylcresol isomers，the number of theoretical plates per meter was around 3000 and the highest operating temperature was 250 ℃. A method for the analysis of m-cresol and p-cresol with high purity was established.

Keywords：neopentyl glycol phthalate polyester；capillary chromatography；cresol isomer；xylenol isomer

化妝品中大麻二酚的檢測方法及溯源研究進(jìn)展

牛可歆¹，趙霞²，廉潔^*1

（1. 中國人民公安大學(xué)偵查學(xué)院，北京 100038；2. 國家毒品實(shí)驗(yàn)室北京分中心，北京 100164）

摘要：大麻二酚（CBD）是大麻的主要成分，因其具有強(qiáng)大的抗炎抗氧、美白保濕等功效，被越來越多地應(yīng)用到化妝品中，但受CBD來源和安全性問題的影響，我國對(duì)其在化妝品領(lǐng)域的應(yīng)用進(jìn)行嚴(yán)格管控。CBD主要通過提取大麻植株中的大麻素獲得，其復(fù)雜的成分和多樣的化妝品品類，使得對(duì)化妝品中CBD的前處理和分析檢測面臨巨大的挑戰(zhàn)。近年來，已開發(fā)出多種化妝品中大麻素的分析方法，液液萃取是最常用的前處理方法，色譜-質(zhì)譜聯(lián)用技術(shù)是首選的檢測方法，同時(shí)便攜式儀器設(shè)備的多種快檢方法也有望應(yīng)用于化妝品中大麻素的檢測。本文綜述了化妝品中CBD前處理和檢驗(yàn)方法的研究進(jìn)展，并結(jié)合CBD的主要來源，探討了基于上述檢驗(yàn)方法的化妝品原料溯源問題，以期為開展相關(guān)科學(xué)研究提供參考和借鑒。

關(guān)鍵詞：大麻二酚；化妝品；色譜-質(zhì)譜聯(lián)用技術(shù)；大麻素；溯源

中圖分類號(hào)：O65    文獻(xiàn)標(biāo)識(shí)碼：A    文章編號(hào)：1000-0720（2023）10-1386-09

Advances of detection methods and traceability study of cannabidiol in cosmetics

NIU Kexin¹，ZHAO Xia²，LIAN Jie^*1

1. School of Investigation，People’s Public Security University of China，Beijing 100038，China；2. Beijing Branch of National Drug Laboratory，Beijing 100164，China）

Abstract：Cannabidiol （CBD） is the main component of cannabis. Because of its powerful anti-inflammatory，antioxidant，whitening and moisturizing effects，it is increasingly used in cosmetics. However，due to the source of CBD and safety issues，China imposes strict controls on its cosmetics sector. CBD in cosmetics mainly comes from extraction of cannabinoids plants. The complexity of its components and the diversity of cosmetic categories make the pretreatment analysis and detection of CBD in cosmetics face huge challenges. In recent years，a variety of analytical methods for detection of cannabinoids in cosmetics have been developed. Liquid-liquid extraction is the most used pretreatment method，and chromatography-mass spectrometry is the preferred laboratory analysis method. With portable instruments and equipment used，a variety of rapid detection methods are also expected to be applied to the detection of cannabinoids in cosmetics. This paper compares the existing detection technologies for detection of cannabinoids in cosmetics，and refers to the idea of chemical typing of cannabis plants，discusses the application of existing detection technologies in the traceability of components，and prospects for the development direction of cannabinoid detection，providing reference for related scientific research.

Keywords：cannabidiol；cosmetics；chromatography-mass spectrometry；cannabinoids；tracing

檢測SARS-CoV-2抗體的電化學(xué)免疫傳感器抗原固定方法研究進(jìn)展

潘藝文¹，王鈺結(jié)¹，陳曉雯¹，張曉敏¹，霍朝暉^*1，2

（1. 廣東第二師范學(xué)院化學(xué)與材料科學(xué)學(xué)院，廣州 510303；2. 廣東省普通高校先進(jìn)材料與節(jié)能減排工程技術(shù)開發(fā)中心，廣州 510303）

摘要：SARS-CoV-2的免疫球蛋白M和G（IgM和IgG）抗體檢測在新型冠狀病毒肺炎（COVID-19）的病情分析和診斷監(jiān)測等方面具有重要意義。電化學(xué)免疫傳感器作為一種高效的檢測工具，可以很好地滿足COVID-19抗體診斷的需求，與傳統(tǒng)的分子學(xué)和血清學(xué)抗體檢測方法相比，表現(xiàn)出優(yōu)異的性能，且具有現(xiàn)場快檢能力。決定電化學(xué)生物傳感器檢測抗體性能的關(guān)鍵技術(shù)是其基底電極的修飾材料和電極表面生物活性分子的固定化技術(shù)。本文以電化學(xué)生物免疫傳感器的設(shè)計(jì)為基礎(chǔ)，綜述了基底電極的修飾材料和功能性生物活性分子在電極表面的固定化方式，并對(duì)未來SARS-CoV-2抗體檢測的電化學(xué)免疫傳感器的研發(fā)進(jìn)行展望，旨在為增強(qiáng)電化學(xué)生物免疫傳感器性能和應(yīng)用價(jià)值提供研究思路。

關(guān)鍵詞：SARS-CoV-2抗體；電化學(xué)；傳感器；構(gòu)建

中圖分類號(hào)：O657.3；G353.11    文獻(xiàn)標(biāo)識(shí)碼：A    文章編號(hào)：1000-0720（2023）10-1395-11

Research progress of antigen fixation methods

 of electrochemical immunosensor for detecting SARS-CoV-2 antibodies

PAN Yiwen¹，WANG Yujie¹，CHEN Xiaowen¹，ZHANG Xiaomin¹，HUO Zhaohui^*1，2

1. School of Chemistry and Materials Science，Guangdong University of Education，Guangzhou 510303，China；2. Engineering Technology Development Center of Advanced Materials & Energy Saving and Emission Reduction in Guangdong Colleges and Universities，Guangzhou 510303，China）

Abstract：The detection of SARS-CoV-2 Immunoglobulin M（IgM） and Immunoglobulin G（IgG） antibodies is of great significance in disease analysis，diagnosis and surveillance of COVID-19. As an highly effective detection tool，electrochemical immunosensors can well meet the needs of COVID-19 antibodies diagnosis. Compared with traditional molecular and serological antibodies detection methods，it shows excellent performance and has the ability of rapid onsite detection. The performance of electrochemical biosensors depends on the modification material on the electrode substrate and the immobilization technology of bioactive molecules on the electrode surface. Based on the design of the electrochemical bioimmunosensors，the immobilization methods of the modification material on the electrode substrate and the functional bioactive molecules on the electrode surface are reviewed，and the development of electrochemical immunosensors for detecting SARS-CoV-2 antibody in the future is prospected，aiming to provide research ideas for enhancing the performance and application of electrochemical bioimmunosensors.

Keywords：SARS-CoV-2 antibody；electrochemistry；sensor；construction

硫化氫中毒檢驗(yàn)技術(shù)研究進(jìn)展

張震¹，張?jiān)品?sup>2，吳小軍^*1，2，王繼芬¹，魯朋武³

（1. 中國人民公安大學(xué)偵查學(xué)院，北京 100038；2. 公安部物證鑒定中心，北京 100038；3. 中國人民公安大學(xué)公安管理學(xué)院，北京 100038）

摘要：硫化氫中毒的檢驗(yàn)鑒定一直都是司法鑒定的難題，大量的硫化氫死亡案件由于檢驗(yàn)方法的缺失導(dǎo)致無法確定死因。本文從硫化氫的物化特性、中毒機(jī)理及代謝、法醫(yī)病理鑒定、毒物檢驗(yàn)等角度進(jìn)行綜述，探究了色譜-質(zhì)譜分析技術(shù)等不同硫化氫檢驗(yàn)方法，總結(jié)出最為合適的硫化氫檢驗(yàn)方法，并對(duì)硫化氫定量及現(xiàn)場檢測進(jìn)行展望，以期為其在司法鑒定領(lǐng)域的研究與應(yīng)用提供參考與借鑒。

關(guān)鍵詞：硫化氫；氣相色譜；液相色譜；質(zhì)譜；分光光度法

中圖分類號(hào)：O65    文獻(xiàn)標(biāo)識(shí)碼：A    文章編號(hào)：1000-0720（2023）10-1406-06

Research progress of detection techniques for hydrogen sulfide poisoning

ZHANG Zhen¹，ZHANG Yunfeng²，WU Xiaojun^*1，2，WANG Jifen¹，LU Pengwu³

1. School of Investigation，People’s Public Security University of China，Beijing 100038，China；2. Physical Evidence Identification Center of Ministry of Public Security，Beijing 100038，China；3. School of Public Security Management，People’s Public Security University of China，Beijing 100038，China）

Abstract：The detection and identification of hydrogen sulfide poisoning is always a difficult problem in judicial identification. In this paper，the physical and chemical characteristics of hydrogen sulfide，poisoning mechanism and metabolism，forensic pathological identification，poison test and other aspects were reviewed，the chromatography-mass spectrometry analysis technology and other different hydrogen sulfide test methods were explored，the most appropriate test method was summarized，quantitative and on-site detection of hydrogen sulfide were expected，aiming to provide reference for its research and application in the field of forensic expertise.

Keywords：hydrogen sulfide；gas chromatography；liquid chromatography；mass spectrometry；spectrophotometry

拉曼光譜技術(shù)在靈敏檢測氣味物質(zhì)中的應(yīng)用進(jìn)展

文有青¹，李芷瑤¹，寧瀅¹，王海霞^*1，2

（1. 天津中醫(yī)藥大學(xué)中藥制藥工程學(xué)院，天津 301617；2. 天津中醫(yī)藥大學(xué)省部共建組分中藥國家重點(diǎn)實(shí)驗(yàn)室，天津 301617）

摘要：氣味物質(zhì)是食品和藥品品質(zhì)評(píng)價(jià)的重要指標(biāo)之一。拉曼光譜技術(shù)，尤其是表面增強(qiáng)拉曼光譜技術(shù)，具有無損、高靈敏、檢測速度快等優(yōu)點(diǎn)，在氣味物質(zhì)靈敏檢測方面具有突出優(yōu)勢。本文總結(jié)和梳理了氣味物質(zhì)化學(xué)結(jié)構(gòu)與拉曼位移之間的關(guān)系，系統(tǒng)綜述了拉曼光譜技術(shù)在甜、苦、酸、鮮和混合氣味物質(zhì)檢測方面中的應(yīng)用，并展望了該技術(shù)在氣味物質(zhì)檢測領(lǐng)域的未來發(fā)展方向。

關(guān)鍵詞：氣味物質(zhì)；表面增強(qiáng)拉曼光譜；快速檢測；靈敏度

中圖分類號(hào)：O657.37    文獻(xiàn)標(biāo)識(shí)碼：A    文章編號(hào)：1000-0720（2023）10-1412-09

Advances of application of Raman spectroscopy for sensitive detection of odor substances

WEN Youqing¹，LI Zhiyao¹，NING Ying¹，WANG Haixia^*1，2

1. College of Pharmaceutical Engineering of Traditional Chinese Medicine，Tianjin University of Traditional Chinese Medicine，Tianjin 301617，China；2. State Key Laboratory of Component-based Chinese Medicine，Tianjin University of Traditional Chinese Medicine，Tianjin 301617，China）

Abstract：Odor is one of the important indexes for the quality evaluation of food and drug. Raman spectroscopy，especially surface enhanced Raman spectroscopy technique，with the advantages of non-destructive，high sensitivity and fast detection speed，has outstanding advantages in the sensitive detection of odor substances. This review summarizes the relationship between the chemical structure of odor and Raman shift，systematically summarizes the application of Raman spectroscopy technique in the detection of sweet，bitter，acid，fresh and mixed odor，and points out the future development direction of this technology in the field of odor detection.

Keywords：odor substances；surfaced enhanced Raman spectroscopy；rapid detection；sensitivity