《分析試驗室》2023年12月第42卷第12期中英文摘要
ZrO2/PPy@玉米芯多孔碳材料的制備及用于檢測稻谷中草甘膦殘留
王惠，何利*
，潘無雙，錢玟，林德賢，劉書亮，陳姝娟
（四川農業大學食品學院，雅安 625014）
摘要：通過在PPy@玉米芯多孔碳修飾的玻碳電極上沉積ZrO2納米粒子，制備了一種靈敏檢測食品中草甘膦殘留的電化學傳感器電極材料。玉米芯多孔碳的平均孔徑為4.07 nm。PPy@玉米芯多孔碳復合材料的高比表面積增加了ZrO2的負載量。PPy@玉米芯多孔碳修飾電極用于草甘膦檢測的線性范圍為0.1~10 μg/kg和10~1000 μg/kg，檢出限為24.4 ng/kg，檢測稻谷中草甘膦的回收率為95.5%~99.1%。該傳感器可用于實際食品樣品中草甘膦殘留的檢測。
關鍵詞：ZrO2/PPy@玉米芯多孔碳；電化學檢測；草甘膦
中圖分類號：O657.1；TB322 文獻標識碼：A 文章編號：1000-0720（2023）12-1563-08
Preparation of ZrO2/PPy@corncobs porous carbon materials for determination of glyphosate residues in rice
WANG Hui，HE Li*，PAN Wushuang，QIAN Wen，LIN Dexian，LIU Shuliang，CHEN Shujuan
College of Food Science，Sichuan Agricultural University，Ya’an 625014，China）
Abstract：A sensing electrode material for sensitive electrochemical detection of glyphosate was prepared by depositing ZrO2 nanoparticles on a glassy carbon electrode modified with PPy@corncob porous carbon. The average pore size of the corncob porous carbon was 4.07 nm. The load of ZrO2 on PPy@corncob was improved due to the high specific area of PPy@corncob porous carbon composite. The linear concentration ranges of this electrode for glyphosate detection was 0.1-10 μg/kg and 10-1000 μg/kg，and the detection limit was 24.4 ng/kg. Meanwhile，the recoveries were 95.5%-99.1% in real sample tests. The electrochemical sensor was proved to be useful for the detection of glyphosate residues in actual food samples.
Keywords：ZrO2/PPy@ corncob porous carbon；electrochemical detection；glyphosate
基于同步熒光與支持向量回歸的典型蔬菜農藥殘留快速檢測
王曉燕，蔣喆臻，馮小濤，郭鑫月，卞海溢，季仁東*
（江蘇省湖泊環境遙感技術工程實驗室，淮陰工學院電子信息工程學院，淮安 223003）
摘要：采用恒波長同步熒光法結合支持向量回歸（SVR）算法，對西紅柿汁中的春雷霉素和多殺菌素農藥殘留含量進行快速檢測。確定了春雷霉素和多殺菌素的最佳波長差（Δλ）分別為70，45 nm，同時得到最佳Δλ下的特征峰分別位于322，292 nm。春雷霉素樣本和多殺菌素樣本的建模結果顯示，2種農藥模型的均方誤差均小于0.002，決定系數（R2）均超過0.99，平均回收率分別為99.5%和100.1%。采用同步熒光結合SVR算法可有效檢測西紅柿中春雷霉素和多殺菌素的含量，并為其它蔬菜中農藥殘留檢測提供方法依據。
關鍵詞：農藥殘留；快速檢測；同步熒光法；支持向量回歸
中圖分類號：O657.3 文獻標識碼：A 文章編號：1000-0720（2023）12-1571-05
Rapid detection of pesticide residues in typical vegetable based on synchronous fluorescence and support vector regression
WANG Xiaoyan，JIANG Zhezhen，FENG Xiaotao，GUO Xinyue，BIAN Haiyi，JI Rendong*
Jiangsu Laboratory of Lake Environment Remote Sensing Technologies，Faculty of Electronic Information Engineering，Huaiyin Institute of Technology，Huai’an 223003，China）
Abstract：A rapid determination method for kasugamycin and spinosad pesticide residues in tomato juice was proposed by the constant wavelength synchronous fluorescence method combined with support vector regression （SVR） algorithm. The optimum wavelength distinctions （Δλ） of kasugamycin and spinosad were 70 and 45 nm，and the optimal characteristic peaks were obtained as 322 and 292 nm，respectively. According to the modelling results of kasugamycin and spinosad samples，the mean square errors of the two pesticide models were less than 0.002，the coefficients of determination （R2） were more than 0.99，and the average recoveries were 99.5% and 100.1%，respectively. The results showed that the synchronous fluorescence combined with SVR method is capable of detecting the contents of kasugamycin and spinosad in tomatoes，and provides a support for the detection of pesticide residues in other vegetables.
Keywords：pesticide residues；rapid detection；synchronous fluorescence；support vector regression
基于摩擦納米發電機的水質檢測
馮朗，龍威*，李萌，向琴，劉文楷
（昆明理工大學機電工程學院，昆明 650500）
摘要：基于接觸起電和靜電感應耦合作用，提出了一種自供電水質檢測技術。通過分析不同液相和固體壁面在摩擦感應過程中電信號的形成輸運機理，明確不同待測水樣通過聚四氟乙烯（PTFE）管道時與壁面形成的摩擦電信號輸出特征，從而實時快速檢測水中無機鹽濃度和雜質成份。結果表明：在摩擦起電過程中，液柱與PTFE管壁之間主要通過電子和帶電粒子形成雙電層的方式在液固界面完成從水相向固相的定向躍遷；隨著液相無機鹽濃度和雜質成份的不同，電極檢測到的感應電勢和電荷密度也呈現不同規律；進一步以去離子水、自來水、礦泉水、紅墨水溶液、聚苯乙烯溶液和不同濃度的無機鹽溶液為例，驗證了其作為液相在摩擦感應過程中形成電信號的差別及其內部組分和開路電壓之間的關系。
關鍵詞：水質檢測；摩擦納米發電機；雙電層；有機物檢測；無機鹽檢測
中圖分類號：X832；TH85 文獻標識碼：A 文章編號：1000-0720（2023）12-1576-08
Water quality detection based on triboelectric nanogenerator
FENG Lang，LONG Wei*，LI Meng，XIANG Qin，LIU Wenkai
Faculty of Mechanical and Electrical Engineering，Kunming University of Science and Technology，Kunming 650500，China）
Abstract：A self-powered water quality detection technology was proposed by coupling contact electrification with electrostatic induction. Through the analysis of the formation and transport mechanism of contact electrification between different liquid phase and solid inner wall phase，triboelectric signal output characteristics of different water samples passed through polytetrafluoroethylene （PTFE） pipes were detected. In this way，the concentrations of inorganic salts and impurities in water can be detected in real time and quickly. The results showed that during the triboelectric process，the directional transition from water to solid phase completed at the liquid-solid interface between the liquid droplet and PTFE pipe wall was mainly through the formation of electric double layer by free electrons and other charged particles. The induced potential and charge density detected by the electrode were various at different concentrations of inorganic salt and impurity composition in the liquid phase. Furthermore，taking deionized water，tap water，mineral water，red ink solution，polystyrene solution and inorganic salt solution with different concentrations as examples，the differences of electrical signals formed in the friction induction process as liquid phase and the relationship between internal components and open-circuit voltage were verified.
Keywords：water quality detection；triboelectric nanogenerator；electric double layer；detection of organic matter；detection of inorganic salt
熒光適配體生物傳感器的構建及用于檢測中藥飲片中的啶蟲脒
張紅艷，陳淑萍，范申，張淑玲，余宇燕*，林舒*
（福建中醫藥大學藥學院，福州 350122）
摘要：構建了一種基于納米金（AuNPs）和碳量子點（CQDs）的熒光適配體傳感方法，并用于啶蟲脒的快速檢測。在優化條件下，熒光強度與啶蟲脒濃度在20~100 μg/mL范圍內具有良好的線性關系，相關系數為0.9972，檢出限為8.31 μg/mL。應用本方法對中藥飲片山藥和太子參中的啶蟲脒進行加標回收實驗，回收率為90.8%~105.7%，相對標準偏差（RSD）為0.4%~5.8%。該方法有望用于啶蟲脒現場快速定量分析。
關鍵詞：熒光生物傳感器；農藥殘留；啶蟲脒；適配體
中圖分類號：O657.31 文獻標識碼：A 文章編號：1000-0720（2023）12-1584-07
Fabrication of fluorescent aptamer sensor for the detection of acetamiprid in Chinese prepared slices of crude drugs
ZHANG Hongyan，CHEN Shuping，FAN Shen，ZHANG Shuling，YU Yuyan*，LIN Shu*
Pharmacy College of Fujian University of Traditional Chinese Medicine，Fuzhou 350122，China）
Abstract：A fluorescent aptamer biosensor based on gold nanoparticles （AuNPs） and carbon quantum dots （CQDs） for the rapid detection of acetamiprid was fabricated. Under the optimized conditions，there was a good linear relationship between the fluorescence intensity and the acetamiprid concentration in the range of 20-100 μg/mL，with a correlation coefficient of 0.9972，and the detection limit was 8.31 μg/mL. This method was applied to the spiked recovery experiment of acetamiprid in traditional Chinese medicine slices of yam and Radix Pseudostellariae，the recoveries ranged from 90.8% to 105.7%，and the relative standard deviations （RSDs） were 0.4%~5.8%. This method is expected to be used for the on site rapidly quantitative analysis of acetamiprid .
Keywords：fluorescent biosensor；pesticide residues；acetamiprid；aptamer
氣相色譜-質譜法檢測紡織品中28種芳香胺和4種芳香胺鹽
劉金源1，2，葉曦雯*2，羅忻2，牛增元2，劉坤2，陳靜2，李晶瑩1
（1. 青島科技大學環境與安全工程學院，青島 266042；2. 青島海關技術中心，青島 266109）
摘要：建立了同時測定紡織品中28種芳香胺和4種芳香胺鹽的氣相色譜-質譜方法。紡織品樣品中偶氮染料和游離態的芳香胺鹽在堿性的檸檬酸鹽緩沖溶液中，經連二亞硫酸鈉還原成芳香胺，經叔丁基甲醚溶劑提取，氣相色譜-質譜法同時測定。優化條件為2 mL 質量分數40%的NaOH堿化、10 mL叔丁基甲醚提取。28種芳香胺均呈良好的線性關系，26種芳香胺線性范圍為0.05~10 mg/L，2，4-二氨基苯甲醚和2，5-二氨基甲苯的線性范圍為0.2~10 mg/L；相關系數為0.996~0.999；26種芳香胺檢出限為0.05 mg/L，2，4-二氨基苯甲醚和2，5-二氨基甲苯的檢出限為0.2 mg/L。2，4-二氨基苯甲醚硫酸鹽的加標回收率為33.1%~36.0%，其余3種芳香胺鹽平均加標回收率為84.5%~124.6%；2，4-二氨基苯甲醚加標回收率為43.7%~64.3%，其余27種芳香胺回收率在71.7%~119.3%之間。陽性樣品檢測結果表明：對于原有芳香胺化合物的檢測，本方法和ISO 14362方法對比無顯著差異；對新增芳香胺特別是2，5-二氨基甲苯，ISO 14362方法存在漏檢風險，而本方法具有更高的回收率。本方法為OEKO-TEX新增的芳香胺及芳香胺鹽的檢測提供了參考。
關鍵詞：氣相色譜-質譜法；芳香胺；芳香胺鹽；紡織品
中圖分類號：O657.63；X832 文獻標識碼：A 文章編號：1000-0720（2023）12-1591-08
Determination of 28 aromatic amines and 4 aromatic amine salts in textiles by gas chromatography-mass spectrometry
LIU Jinyuan1，2，YE Xiwen*2，LUO Xin2，NIU Zengyuan2，LIU Kun2，CHEN Jing2，LI Jingying1
1. College of Environmental and Safety Engineering，Qingdao University of Science and Technology，Qingdao 266042，China；2. Technology Center of Qingdao Customs，Qingdao 266109，China）
Abstract：A method for the detection of 28 aromatic amines and 4 aromatic amine salts in textiles by gas chromatography-mass spectrometry was established. Azo dyes and free aromatic amine salts in textiles were reduced to aromatic amines by sodium dithionite in alkaline citrate buffer solution，extracted by tert-butyl methyl ether solvent，and then determined simultaneously by gas chromatography-mass spectrometry. The optimized pretreatment conditions were alkalized by 2 mL of 40% NaOH and extracted by 10 mL of tert butyl methyl ether. 28 aromatic amines showed good linear relationships，the linear ranges were 0.05-10 mg/L for 26 aromatic amines，and 0.2-10 mg/L for 2，4-diaminoanisole and 2，5-diaminotoluene，with the correlation coefficients of 0.996-0.999. The detection limits were 0.05 mg/L for 26 aromatic amines，and 0.2 mg/L for 2，4 diaminoanisole and 2，5-diaminotoluene. The standard adding recovery experiments showed that the recoveries of 2，4-diaminoanisole sulfate were 33.1%-36.0%，and that of the other three aromatic amine salts were 84.5%- 124.6%. The recoveries of 2，4-diaminoanisole were 43.7%-64.3%，and that of the other 27 aromatic amine were 71.7%-119.3%. The test results of positive samples showed that there was no significant difference between this method and ISO 14362 method for the detection of original aromatic amine compounds. For newly added aromatic amines，especially 2，5-diaminotoluene，the ISO 14362 method has the risk of missing detection，while this method has a higher recovery rate，and can provide a reference for the detection of newly added aromatic amines and aromatic amine salts in OEKO-TEX.
Keywords：gas chromatography-mass spectrometry；aromatic amines；aromatic amine salts；textiles
基于雙頻超聲輔助酶解結合EDTA法快速高效提取水產品中的鉛
朱念辛，郝麗玲，劉馨娜，黃椿華，顏會銘，諸子蘅，蔡欣怡，徐斐*
（上海理工大學健康科學與工程學院，上海 200093）
摘要：建立了一種基于雙頻超聲輔助酶解（DUED）結合乙二胺四乙酸二鈉鹽（EDTA）提取水產品中鉛的前處理方法。該方法利用超聲探頭的空化效應促進蛋白酶的水解進程，并結合EDTA的強絡合能力，可在12 min內快速提取魚肉粉中的鉛。通過單因素實驗考察料液比、酶配方、酶解時間、EDTA提取時間和EDTA濃度對鉛提取率的影響。在雙頻超聲與EDTA提取相結合的模式下，最佳提取條件為：pH 7.0的磷酸鹽溶液為緩沖溶液，料液比為1∶6 （700 mg魚肉粉樣品+4.2 mL磷酸鹽緩沖液），10 mg風味蛋白酶（5.5×104 U/g）與70 mg中性蛋白酶（18.3×105 U/g）為復配酶，超聲輔助酶解時間為6 min，EDTA濃度為40 mmol/L，提取時間6 min。在最優條件下，魚肉粉中鉛的提取率可達（84.83±1.00）%。該前處理方法可實現魚肉粉中鉛的快速、高效提取，且與重金屬的快速檢測方法具有良好的兼容性，是一種有前景的食品安全檢測前處理技術。
關鍵詞：雙頻超聲輔助酶解；乙二胺四乙酸二鈉鹽；鉛；水產品；前處理
中圖分類號：TS254.7 文獻標識碼：A 文章編號：1000-0720（2023）12-1599-07
A rapid and efficient extraction method for lead from aquatic products by dual-frequency ultrasonic-assisted enzymatic digestion combined with EDTA
ZHU Nianxin，HAO Liling，LIU Xinna，HUANG Chunhua，YAN Huiming，ZHU Ziheng，CAI Xinyi，XU Fei*
School of Health Science and Engineering，University of Shanghai for Science and Technology，Shanghai 200093，China）
Abstract：Herein，a pretreatment method based ondual-frequency ultrasonic-assisted enzymatic digestion （DUED） combined with disodium ethylenediaminetetraacetate （EDTA） for extracting lead from aquatic products was established. In this method，the cavitation effect of ultrasonic probe was employed to promote the hydrolysis process of protease，and combined with the strong complexing ability of EDTA，the lead in fish meal was quickly extracted within 12 min. The single factor experiment was carried out to investigate the effects of solid-liquid ratio，enzyme dosage，enzymolysis time，EDTA extraction time and concentrations on the extraction efficiency of lead. Under the mode of combining dual frequency ultrasound with EDTA extraction，the optimal extraction conditions were exhibited as follows：phosphate solution （pH 7.0） as buffer solution，solid-liquid ratio of 1∶6 （700 mg of fish meal sample with 4.2 mL of phosphate buffer solution），10 mg of flavor protease （5.5×104 U/g） and 70 mg of neutral protease （18.3×105 U/g） as complex enzyme formula，40 mmol/L EDTA as extractant. The extraction rate of the lead from fish meal was around （84.83±1.00）% within 12 min，of which 6 min for DUED and 6 min for EDTA extraction. The results showed that the pretreatment method could achieve rapid and efficient extraction of lead from fish meal，and possesses favourable compatibility with the rapid determination of heavy metal. It can be recognized as a promising pretreatment technology for food safety detection.
Keywords：dual-frequency ultrasound-assisted enzymeextraction；ethylenediaminetetraacetic acid disodium salt；lead；aquatic products；pretreatment
基于核酸適體的試紙條檢測三磷酸腺苷
任林嬌1，王朋偉1，陳青華*1，齊汝賓1，閆艷霞2，張培1，秦自瑞1，陳高凱1，姜利英*1，3
（1. 鄭州輕工業大學電氣信息工程學院，鄭州 450002；2. 鄭州輕工業大學計算機與通信工程學院，鄭州 450002；3. 鄭州輕工業大學量子科技研究院，鄭州 450002）
摘要：將核酸適體（Aptamer）的特異性與納米金顆粒的獨特光學性質相結合，制備了一種適用于小分子檢測的干式試紙條。該試紙條以修飾功能化核酸適體（PloyT13-Aptamer）的納米金為識別元件，在控制線（C）上修飾ployA13序列，與識別元件結合以判斷試紙條的有效性；在測試線（T）上修飾與Aptamer部分互補的DNA序列，與待測物形成競爭關系，通過T線上納米金顯色的深淺來定性或定量分析待測物濃度。結果表明，優化實驗條件下，觀察T線顏色變化可實現三磷酸腺苷（ATP）的肉眼定性檢測，視覺檢出限為10 μmol/L。使用Image J軟件進行定量分析，試紙條檢測范圍為10~1000 μmol/L，檢出限為2.4 μmol/L。該試紙條生物傳感器可以在10 min內得出檢測結果且特異性良好，血清中回收率為104.4%~119.0%，為ATP的現場快速檢測提供了一種經濟有效的方法。
關鍵詞：試紙條；核酸適體；納米金顆粒；三磷酸腺苷
中圖分類號：O657.3 文獻標識碼：A 文章編號：1000-0720（2023）12-1606-09
Determination of adenosine triphosphate by aptamer strips
REN Linjiao1，WANG Pengwei1，CHEN Qinghua*1，QI Rubin1，YAN Yanxia2，ZHANG Pei1，QIN Zirui1，CHEN Gaokai1，JIANG Liying*1，3
1. College of Electrical and Information，Zhengzhou University of Light Industry，Zhengzhou 450002，China；2. College of Computer and Communication Engineering，Zhengzhou University of Light Industry，Zhengzhou 450002，China；3. Academy for Quantum Science and Technology，Zhengzhou University of Light Industry，Zhengzhou 450002，China）
Abstract：A dry strip for small molecule detection was prepared by combining specific aptamers and gold nanoparticles （AuNPs） with unique optical properties. The ployA13 sequence was modified on the control line （C） and the PloyT13-Aptamer nanogold was used as the recognition element to judge the validity of the strip. The DNA sequence complementary to aptamer was modified on the test line （T） to form a competitive relationship with the object to be tested. The concentrations of the target is capable of being analyzed qualitatively and quantitatively by the color shade of the AuNPs on the T line. The results exhibited that the color change of the T-line can be observed under optimized conditions，and the visual detection limit of ATP was 10 μmol/L. The detection range of the strip was 10-1000 μmol/L with a detection limit of 2.4 μmol/L，when Image J software was used for quantitative analysis. The strip biosensor can produce results within 10 min with excellent specificity，and the serum recovery rates were 104.4%-119.0%，which provides an economical and effective strategy for rapid detection of ATP in relevant fields.
Keywords：test strip；aptamer；gold nanoparticles；adenosine triphosphate
水溶性糖基熒光探針用于肝癌細胞的靶向標記
譚名超，劉芳美，沈瓊霞，厲凱彬*
（臺州學院醫藥化工學院，臺州 318000）
摘要：以羅丹明熒光團作為骨架，通過點擊化學的方法引入半乳糖基，設計合成了一種具備肝癌細胞靶向功能的熒光探針Glycosyl Rhodamine（GR）。糖基的引入，使得探針具有較好的水溶性和生物靶向性。在分子溶液水平測試了探針GR的紫外和熒光光譜，發現探針GR對Hg2+選擇性良好，其它金屬陽離子無干擾，并具備較好的濃度依賴關系。利用核磁滴定實驗研究了探針與Hg2+的響應機理。細胞毒性實驗表明，探針GR具有良好的生物相容性，當探針濃度高達100 μmol/L時，細胞存活率大于100%。基于探針分子內半乳糖對肝癌細胞表面糖蛋白受體的特異性識別，利用 Hg2+的配位作用，實現了HepG2肝癌細胞的靶向標記。
關鍵詞：糖基熒光探針；肝癌細胞；汞離子；羅丹明
中圖分類號：O657.32 文獻標識碼：A 文章編號：1000-0720（2023）12-1615-07
Water-soluble glycosyl fluorescent probe for targeting labelling of hepatoma cells
TAN Mingchao，LIU Fangmei，SHEN Qiongxia，LI Kaibin*
Department of Chemistry，Taizhou University，Taizhou 318000，China）
Abstract：A fluorescence probe of Glycosyl Rhodamine （GR） with the function of liver cancer cells targeting was developed. The rhodamine fluorophore was used as the skeleton coupled，and the contained galactose group was introduced via click chemistry method. The introduction of glycogroup promoted the water solubility and biological targeting of the probe. The ultraviolet and fluorescence spectra of the probe GR were tested at the molecular level. The probe GR possessed favorable selectivity to Hg2+ with good concentration dependence，and the interference of other metal cations was limited to it. The response mechanism between GR and Hg2+ was studied by NMR titration. The cytotoxicity test showed that the probe GR owned satisfactory biocompatibility，and the cell viability was more than 100% when the probe concentration was 100 μmol/L. Based on the specific recognition of the glycoprotein receptor on the surface of hepatocellular carcinoma cells by galactose within the probe molecule，the targeted labeling of HepG2 hepatocellular carcinoma cells was realized by the coordination of Hg2+.
Keywords：glycosyl fluorescent probe；liver cancer cells；mercury ion；Rhodamine
酸水解-酶水解-UPLC-MS/MS測定特殊醫學用途配方食品中多種氨基酸和牛磺酸
盧蘭香，薛霞，張艷俠，孫立臻，程志，鄭文靜，鄭紅，宿書芳，尹麗麗，劉艷明*，王駿，祝建華
（山東省食品藥品檢驗研究院，山東省食品藥品安全檢測工程技術研究中心，山東省特殊醫學用途配方食品質量控制工程技術研究中心，濟南 250101）
摘要：利用酸水解與酶水解互補，采用超高效液相色譜-串聯質譜法（UPLC-MS/MS），建立了特殊醫學用途配方食品中22種氨基酸和牛磺酸的檢測方法。樣品經酸水解或酶水解提取，采用6-氨基喹啉基-N-羥基琥珀酰亞胺-氨基甲酸酯（AQC）衍生后，以乙腈-甲酸銨（10 mmol/L）為流動相梯度洗脫，通過AccQ-Tag Ultra C18色譜柱進行分離，三重四極桿質譜電噴霧多反應監測模式檢測，內標法定量。結果表明：22種氨基酸和牛磺酸線性關系良好，相關系數均大于0.9956；檢出限在0.0028~0.0225 g/100 g之間，定量限在0.0094~0.0751 g/100 g之間。22種氨基酸和牛磺酸的平均加標回收率在90.1%~104.7%之間，相對標準偏差在1.1%~4.3%之間。該方法實現了GB 29922-2013和GB 25596-2010中規定的22種不同性質氨基酸以及牛磺酸成分的水解提取與準確測定，適用于特殊醫學用途配方食品中氨基酸和牛磺酸的準確定性、定量分析。
關鍵詞：氨基酸；牛磺酸；水解；衍生；特殊醫學用途配方食品；超高效液相色譜-串聯質譜法
中圖分類號：TS207.3 文獻標識碼：A 文章編號：1000-0720（2023）12-1622-09
Determination of amino acids and taurine in formula foods for special medical by UPLC-MS/MS with acidic hydrolysis and enzymatic hydrolysis
LU Lanxiang，XUE Xia，ZHANG Yanxia，SUN Lizhen，CHENG Zhi，ZHENG Wenjing，ZHENG Hong，SU Shufang，YIN Lili，LIU Yanming*，WANG Jun，ZHU Jianhua
Shandong Institute for Food and Drug Control，Shandong Research Center of Engineering and Technology for Safety Inspection of Food and Drug，Shandong Research Center of Engineering and Technology for Quality Control of Food for Special Medical Purposes，Jinan 250101，China）
Abstract：A simultaneous determination method for 22 amino acids and taurine in formula foods for special medical purpose by ultra-high performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS） with the complementary technology of acidic hydrolysis and enzymatic hydrolysis was established. The samples were extracted by acidic hydrolysis or enzymatic hydrolysis，and the perpared analytes were derivatized with 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate （AQC）. The chromatographic separation was carried out using AccQ-Tag Ultra C18 column，with gradient elution using a mobile phase consisting of acetonitrile and ammonium formate （10 mmol/L）. The target compounds were detected by triple quadrupole mass spectrometry with electrospray ionization （ESI） under the multiple reaction monitoring （MRM） mode，and then quantified by an internal standard method. Calibration curves had satisfactory linearities for 22 amino acids and taurine，and the correlation coefficients were above 0.9956. The limits of detection were in the range of 0.0028-0.0225 g/100 g，and the limits of quantitation were in the range of 0.0094-0.0751 g/100 g. The average recoveries were from 90.1% to 104.7%，and the relative standard deviations ranged from 1.1% to 4.3%. The method realized the hydrolytic extraction and accurate determination of 22 amino acids and taurine in GB 29922-2013 and GB 25596-2010. This method is suitable for accurate qualitative and quantitative analysis of amino acids and taurine in formula foods for special medical purpose.
Keywords：amino acids；taurine；hydrolysis；derivatization；food for special medical purposes；ultra-high performance liquid chromatography-tandem mass spectrometry
雞蛋中氟苯尼考時間分辨熒光快速定量檢測卡的制備和應用
余文琴*1，龔迎昆1，李姍1，史沁芳1，肖昭競1，李明偉2，章健2
（1. 重慶市計量質量檢測研究院，重慶 401123；2. 成都微瑞生物科技有限公司，成都 611731）
摘要：制備了一種可快速定量檢測氟苯尼考的時間分辨熒光免疫層析卡，并建立了一種快速定量檢測雞蛋中氟苯尼考的時間分辨熒光免疫層析方法。采用時間分辨熒光微球標記氟苯尼考單抗，篩選了具有高靈敏度和特異性的氟苯尼考抗原抗體，優化了時間分辨熒光微球與氟苯尼考單抗的標記條件、氟苯尼考抗原在硝酸纖維（NC）膜上的包被濃度、稀釋復溶液配方等條件。結果表明：氟苯尼考的線性范圍為0.05~1.00 μg/kg，檢出限為0.05 μg/kg。采用雞蛋進行加標回收實驗，氟苯尼考的回收率在85.0%~98.0%，批內相對標準偏差（RSD）為8.0%~12%，批間RSD為11%~17%。實際樣品的檢測結果與國標方法結果無顯著性差異。方法適用于雞蛋中氟苯尼考的現場快速定量篩查。
關鍵詞：氟苯尼考；時間分辨；熒光免疫層析；快速定量檢測
中圖分類號：O657.3；TS201.6 文獻標識碼：A 文章編號：1000-0720（2023）12-1631-07
Preparation and application of a time-resolved fluorescence rapid quantitative detection card for the determination of florfenicol in eggs
YU Wenqin*1，GONG Yingkun1，LI Shan1，SHI Qinfang1，XIAO Zhaojing1，LI Mingwei2，ZHANG Jian2
1. Chongqing Academy of Metrology and Quality Inspection，Chongqing 401123，China；2.Chengdu Weirui Biotechnology Co. Ltd.，Chengdu 611731，China）
Abstract：A method based on a developed time-resolved immunochromatogram card was proposed for rapid quantitative detection of flufenicol in eggs. Flufenicomumab was labeled with time-resolved fluorescent microspheres and the Fflufenicol antigens with high sensitivity and specificity were screened. The labeling conditions of time-resolved fluorescent microspheres and flufenicomumab，the coating concentrations of flufenicomumab antigen on nitrate-fiber membrane （NC），and the formulation of diluted complex solution were optimized，respectively. The results showed that the linear range for the flufenicol was 0.05-1.00 μg/kg，and the detection limit was 0.05 μg/kg. The spiked recoveries of florfenicol were 85.0%-98.0%，the intra-batch relative standard deviations （RSDs） were 8.0%-12%，and the inter-batch RSDs were 11%-17%. The difference of the test results of actual samples between this method and the national standard method is little. The developed rapid time-resolved fluorescence determination method is suitable for the rapid and quantitative screening of flurfenicol in eggs.
Keywords：flufenicol；time-resolved；fluorescence immunochromatography；rapid quantitative detection
基于SERRS法檢測鹽酸普魯卡因
胡振帥1，李文杰1，趙超陽1，臧佳琳2，劉婷婷1，王慧玉1，付雙1，黃鑫睿1，隋會敏*1
（1. 齊齊哈爾醫學院藥學院，齊齊哈爾 161000；2. 齊齊哈爾醫學院附屬第二醫院，齊齊哈爾 161000）
摘要：結合偶氮衍生反應，建立了鹽酸普魯卡因的表面增強共振拉曼散射（SERRS）檢測方法。將對巰基苯胺（PATP）重氮化，得到的重氮鹽離子與鹽酸普魯卡因發生偶氮衍生反應，生成相應偶氮產物，再與銀納米粒子混合并立即進行拉曼測試，最后利用偶氮產物的SERRS響應檢測鹽酸普魯卡因含量。優化實驗條件為：最大吸收峰波長為442 nm的銀溶膠作為增強基底，532 nm作為激發波長，偶氮衍生的最佳時間為20 min，偶氮衍生過程中最佳Na2CO3質量濃度為8%。在10 ng/mL~10 μg/mL范圍內，得到SERRS強度比值I1435/I384（y）與鹽酸普魯卡因濃度負對數（x）間的線性方程為y=78.97421-8.66853x，線性相關系數R2為0.9774，檢出限（LOD）為8.196 ng/mL。方法對鹽酸普魯卡因注射液測定結果與標準值基本一致，采用標準加入法測得回收率在96.4%~103.3%之間，相對標準偏差（RSD）在3.4%~6.4%之間。將方法用于大鼠血清模擬樣品測定，回收率在96.0%~103.5%之間，RSD在4.3%~7.6%之間，為監管鹽酸普魯卡因非法添加和濫用提供方便快捷且可靠的檢測方法。
關鍵詞：表面增強共振拉曼散射（SERRS）；普魯卡因；偶氮；檢測
中圖分類號：O657.37 中獻標識碼：A 文章編號：1000-0720（2023）12-1638-06
Determination of procaine hydrochloride based on SERRS
HU Zhenshuai1，LI Wenjie1，ZHAO Chaoyang1，ZANG Jialin2，LIU Tingting1，WANG Huiyu1，FU Shuang1，HUANG Xinrui1，SUI Huimin*1
1. School of Pharmacy，Qiqihar Medical University，Qiqihar 161000，China；2. The Second Affiliated Hospital of Qiqihar Medical University，Qiqihar 161000，China）
Abstract：A simple and sensitive surface-enhanced resonant Raman scattering （SERRS）method for the determination of procaine hydrochloridewas established by combining with azo derivatization. The dizaonium ions from p-aminothiophenol （PATP） reacted with procaine hydrochloride via azo coupling reaction. Then the generated azo product was mixed with silver nanoparticles for immediate Raman measurements. The concentration of procaine hydrochloride can be determined through SERRS response of azo product. The optimum conditions of the derivatization process were as followed：silver sol with the maximum absorption of 442 nm was used as enhancing substrate，and the 532 nm utilized as excitation wavelength，the azoderivatization time was 20 min，the concentration of sodium carbonate was 8%. The linear equation between I1435/I384 and the negative logarithm of procaine hydrochloride concentration was y=78.97421-8.66853x，with the correlation coefficient （R2） of 0.9774 in the range from 10 ng/mL to 10 μg/mL. The limit of detection （LOD） was 8.196 ng/mL. The determination results of procaine hydrochloride injection were basically consistent with the standard values. The recoveries were 96.4%-103.3%，and the RSDs were 3.4%-6.4% by standard addition method. The method was additionally applied to the determination of rat serum simulated samples. The recoveries were 96.0%-103.5%，and the RSDs were 4.3%-7.6%. The method is simple and sensitive，providing a convenient，fast and reliable detection way to the supervision of illegal addition and the abuse of procaine hydrochloride.
Keywords：surface-enhanced resonance Raman scattering （SERRS）；procaine；azo；detection
人體呼出氣體一氧化氮的氣液相化學發光檢測
熊椏林1，毛婭2，黃丹3，范力瑞1，付大友1，譚文淵*1，張歡1，吳雨燃1
（1. 四川輕化工大學化學工程學院，自貢 643000；2. 四川化工職業技術學院藥品與環境工程學院，瀘州 646009；3. 瀘州市應急保障中心，瀘州 646000）
摘要：通過選擇KMnO4氧化劑將NO氣體氧化為NO2氣體，基于魯米諾（Luminol）化學發光檢測NO2氣體的體系，采用自主研發的氣液相化學發光檢測儀，建立了一種化學發光檢測呼吸系統疾病中痕量NO氣體的方法。研究了KMnO4濃度，pH以及Luminol檢測NO2體系中各組分濃度對化學發光強度的影響。結果表明，在KMnO4濃度為0.15 mol/L、pH 1.7時氧化效果最好，在Luminol（5.0 mmol/L）、KOH（50 mmol/L）體系中加入Na2SO3（0.10 mol/L）、乙二醇（3.0%（V/V））能顯著增強Luminol體系檢測NO2的化學發光信號。最優條件下，在10~250 μg/L范圍內，NO濃度與發光強度呈現出良好的線性關系。
關鍵詞：氣液相化學發光；一氧化氮；魯米諾；呼吸系統疾病
中圖分類號：O659.21 文獻標識碼：A 文章編號：1000-0720（2023）12-1644-05
Gas-liquid phase chemiluminescence detection of human exhaled gas nitric oxide
XIONG Yalin1，MAO Ya2，HUANG Dan3，FAN Lirui1，FU Dayou1，TAN Wenyuan*1，ZHANG Huan1，WU Yuran1
1. School of Chemical Engineering，Sichuan University of Science and Engineering，Zigong 643000，China；2. School of Pharmaceutical Products and Environmental Engineering，Sichuan Vocational College of Chemical Technology，Luzhou 646009，China；3. Luzhou City Emergency Support Center，Luzhou 646000，China）
Abstract：A chemiluminescence method for the detection of trace level of NO gas in respiratory diseases was established by a self-developed gas-liquid chemiluminescence detector，which the main mechanism was based on KMnO4 oxidizing NO to NO2 and generating chemiluminescence signal. The influence of the concentration of KMnO4，pH and Luminol on the chemiluminescence intensity in NO2 system were investigated. The oxidation effect was optimal at the KMnO4 concentration of 0.15 mol/L and pH value of 1.7. Meanwhile，the additions of Na2SO3 （0.10 mol/L） and ethylene glycol （3%） in the Luminol （5.0 mmol/L） and the KOH （50 mmol/L） can significantly enhance the intensity of luminol system. Under the optimal conditions，the NO concentration showed a favorable linear relationship with the luminescence intensity in the range of 10-250 μg/L. This method possessed multiple benefits like high accuracy，good stability，easy carrying and green environmental protection.
Keywords：gas-liquid phase chemiluminescence；nitric oxide；luminol；respiratory disease
基于智能手機檢測系統的抗壞血酸電化學傳感應用
汪廣源1，張兆康2，陳芳如2，李艷霞*2
（1. 福州大學環境與安全工程學院，福州 350108；2. 閩江學院材料與化學工程學院，福州 350108）
摘要：制備了一種基于石墨烯微電極的抗壞血酸（AA）智能傳感器。通過設計與U盤式電化學分析儀相兼容的直插式三電極圖案，采用激光直寫技術制備圖案化石墨烯電極，選擇AA作為目標分析物，構建了一種基于石墨烯微電極的AA便攜式智能檢測方法。使用PalmSens U盤式微型電化學分析儀，結合智能手機APP檢測，采用循環伏安法，考察了所制備的石墨烯電極對AA的電化學響應。結果表明，pH 1時，在AA濃度0.01~0.5 mg/mL范圍內，峰電流與AA濃度具有良好的線性關系。所設計的石墨烯微電極可兼容于PalmSens U盤式電化學分析儀，所構建的檢測方法可用于汗液、尿液等不同生物樣品的檢測。
關鍵詞：PalmSens U盤式電化學分析儀；石墨烯；激光直寫；抗壞血酸
中圖分類號：R857.3 文獻標識碼：A 文章編號：1000-0720（2023）12-1649-06
Application of ascorbic acid electrochemical sensing based on smart phone detection system
WANG Guangyuan1，ZHANG Zhaokang2，CHEN Fangru2，LI Yanxia*2
1. College of Environment and Safety Engineering，Fuzhou University，Fuzhou 350108，China；2. College of Materials and Chemical Engineering，Minjiang University，Fuzhou 350108，China）
Abstract：An intelligent sensor of ascorbic acid （AA） based on graphene microelectrode was constructed. By designing the pattern of a three-electrode system which is compatible with the U-disk electrochemical analyzer，a portable intelligent detection method for AA was developed based on graphene microelectrode using laser direct writing technology. The electrochemical response of the prepared graphene electrode to AA was assessed by cyclic voltammetry through smart phone detection. The results showed that the concentration of AA had a good linear relationship in the range of 0.01-0.5 mg/mL at pH 1. The designed graphene microelectrode is compatible with the PalmSens U-disk electrochemical analyzer. The prepared method can be used for the detection of sweat and urine samples.
Keywords：palmsens U-disk electrochemical analyzer；graphene；laser direct writing；ascorbic acid
分壓校正頂空氣相色譜法測定重晶石礦總有機質含量
劉學琰，李偉，于康，范智禹，羅迎春，戴毅*
（貴州民族大學化學工程學院，貴陽 550025）
摘要：建立了一種分壓校正頂空氣相色譜測定重晶石礦中總有機質含量的新方法。酸性條件下，K2Cr2O7將礦樣中的有機質氧化為CO2，通過分壓校正可知頂空瓶中CO2和O2的信號值之比α與有機質含量呈正相關。因此可通過檢測α測定重晶石樣品中的有機質含量。結果表明，在120 ℃下加熱10 min，重晶石礦樣品與K2Cr2O7溶液（0.136 mol/L）的反應達到平衡。總有機質含量與α值之間存在很好的線性關系，相關系數（R2）為0.999，相對標準偏差（RSD）<2.9%，加標回收率在95.6%~109.2%之間，定量限為0.018%。本方法適用于重晶石礦中有機質含量的批量檢測。
關鍵詞：重晶石礦；頂空氣相色譜法；有機質含量
中圖分類號：O657.7 文獻標識碼：A 文章編號：1000-0720（2023）12-1655-05
Determination of the total organic matter content in barite ore by partial- pressure-corrected headspace gas chromatography
LIU Xueyan，LI Wei，YU Kang，FAN Zhiyu，LUO Yingchun，DAI Yi*
School of Chemical Engineering，Guizhou Minzu University，Guiyang 550025，China）
Abstract：A method for determining the total organic matter content in barite ore using partial-pressure-corrected headspace gas chromatography was constructed. The organic matter in barite ore was oxidized to CO2 by K2Cr2O7 under acidic condition，and the ratio of CO2 and O2 signals in headspace vial was positively correlated with the content of organic matter by partial pressure-corrected method. Therefore，the content of organic matter in barite samples can be determined by measuring α value. The results showed that barite sample could react completely with K2Cr2O7 solution （0.136 mol/L） at 120 ℃ for 10 min. A good linearity between the total organic matter content and the α value was obtained （R2=0.999），with the relative standard deviation less than 2.9%，the recoveries ranged from 95.6% to 109.2%，and the limit of quantitation was 0.018%. This method can be used for batch determination of organic matter content in barite ore.
Keywords：barite ore；headspace gas chromatography；total organic matter content
基于Mn2+增強的氧化石墨烯熒光開關和雜交鏈式反應信號放大的新型納米傳感器高靈敏檢測作物轉基因
褚秀玲1，梅如波1，隋本會1，李凱1，張川1，朱德頌*2
（1. 山東省泰安生態環境監測中心，泰安 271000；2. 山東農業大學化學與材料科學學院，泰安 271018）
摘要：開發了一種新型納米傳感器，利用Mn2+增強的石墨烯（GO）熒光開關（Mn2+-GO-FS）結合雜交鏈式反應（HCR）進行信號放大，用于作物中Bt轉基因的高靈敏檢測。本傳感器利用Mn2+-GO-FS作為HCR發夾探針載體，在Mn2+的輔助下快速吸附發夾探針，進而淬滅探針上標記的熒光基團（FAM），獲得最低的背景信號。目標Bt轉基因作為觸發器，啟動2種亞穩態發夾探針（H1和H2）之間的級聯雜交事件，聚合成缺口長雙螺旋結構（dsDNA），由于GO對dsDNA的吸附能力較弱，dsDNA脫離GO表面，產生更強的熒光。經HCR信號放大后的檢測結果符合預期。最佳條件下，體系的熒光強度與Bt基因濃度在0.1 pmol/L~50 nmol/L范圍內呈線性關系，檢出限0.05 pmol/L。該傳感器具有良好的選擇性和檢測實際樣品的潛力。
關鍵詞：Mn2+；氧化石墨烯熒光開關；雜交鏈式反應信號放大；高靈敏檢測；Bt轉基因
中圖分類號：O657.3 文獻標識碼：A 文章編號：1000-0720（2023）12-1660-06
A novel nanosensor based on Mn2+-enhanced graphene oxide fluorescence switch and hybrid chain reaction signal amplification for highly sensitive detection of crop transgene
CHU Xiuling1，MEI Rubo1，SUI Benhui1，LI Kai1，ZHANG Chuan1，ZHU Desong*2
1. Shandong Tai'an Ecological Environment Monitoring Center，Tai'an 271000，China；2. School of Chemistry and Materials Science，Shangdong Agricultural University，Tai'an 271018，China）
Abstract：A simple，enzyme-free，and high-sensitivity novel nanosensor was developed by utilizing manganese ion （Mn2+）-enhanced graphene oxide （GO） fluorescence switch （Mn2+-GO-FS） which was combined with hybridization chain reaction （HCR） for signaling amplified and highly sensitive detection of Bt transgene in crops. This sensor utilized Mn2+-GO-FS as the HCR hairpin probes carrier and rapidly adsorbed the hairpin probes with the assistance of Mn2+，which efficiently quenched the fluorophores （FAM） labeled on the probe to obtain the lowest background signal. The target Bt transgene acted as a trigger to initiate a cascade of hybridization events between two metastable hairpin probes （H1 and H2） to aggregate into a gap-long duplex structure （dsDNA）. Because of the weak adsorption of GO to dsDNA，dsDNA detached from the GO surface，resulting in stronger fluorescence. The detection results after HCR signal amplification were encouraging. Under the optimal conditions，the fluorescence intensity was linearly related to its concentration in the range of 0.1 pmol/L-50 nmol/L，and the detection limit was 0.05 pmol/L，indicating the sensor had good selectivity and potential to detect real samples.
Keywords：Mn2+；Mn2+-GO-FS；hybrid chain reaction signal amplification；highly sensitive detection；Bt transgene
基于Fe3O4@SiO2@Ag/GCE傳感器檢測土霉素
賈榮玲*，裴瑞杰，李生濤，王桂楨
（河南省動物疫病防控工程技術研究中心，南陽農業職業學院牧醫工程學院，南陽 473000）
摘要：合成了具有核殼結構的Fe3O4@SiO2納米復合材料，在Fe3O4@SiO2表面負載銀納米離子，制備了一種新型的Fe3O4@SiO2@Ag復合材料，并采用玻碳電極（GCE）構建Fe3O4@SiO2@Ag/GCE傳感器，對土霉素（OTC）進行定量檢測。優化了電解質溶液的種類和pH，Fe3O4@SiO2@Ag用量以及富集時間和富集電位等實驗條件。在最佳條件下，OTC濃度（c）與峰電流（Ip）在0.01~120 μmol/L范圍內呈線性關系，線性方程為Ip=0.9307c-0.0033，線性相關系數R2=0.9986，檢出限為8.2 nmol/L。該傳感器對牛奶中OTC的檢測結果與國標法結果一致。
關鍵詞：四氧化三鐵；銀；納米復合材料；土霉素；電化學傳感器
中圖分類號：TS207.3 文獻標識碼：A 文章編號：1000-0720（2023）12-1666-07
Detection of oxytetracycline based on Fe3O4@SiO2@Ag/GCE sensor
JIA Rongling*，PEI Ruijie，LI Shengtao，WANG Guizhen
Henan Engineering and Technology Research Center for Animal Disease Prevention and Control，Nanyang Vocational College of Agriculture of Veterainary Medicine and Engineering，Nanyang 473000，China）
Abstract：The Fe3O4@SiO2 nanocomposite with core-shell structure was synthesized. A new type of nanocomposite Fe3O4@SiO2@Ag was prepared by loading silver nanoparticles on the surface of Fe3O4@SiO2，and a Fe3O4@SiO2@Ag/GCE sensor was constructed using glassy carbon electrode （GCE） to detect oxytetracycline （OTC）. The type and pH of electrolyte solution，the amount of Fe3O4@SiO2@Ag，the enrichment time and enrichment potential were optimized，respectively. Under the optimal conditions，the OTC concentration （c）and peak current （Ip） had a linear relationship in the concentration range of 0.01-120 μmol/L，and the equation was Ip=0.9307c-0.0033，with the coefficient R2=0.9986. The detection limit was 8.2 nmol/L. The detection results of OTC in milk by this method were consistent with that of national standard method.
Keywords：ferric oxide；silver；nanocomposites；oxytetracycline；electrochemistry；sensor
膠束毛細管電泳同時分離測定葛根及其制劑中的5種異黃酮
張春莉，郭愛琳，曹秋娥，李菲*
（云南大學化學科學與工程學院，昆明 650091）
摘要：建立了一種新的膠束毛細管電泳方法，用于同時分離檢測葛根素、大豆苷、3'-甲氧基葛根素、3'-羥基葛根素和4'-甲氧基葛根素5種異黃酮。優化的實驗條件為：以40 mmol/LNa2B4O7+4 mmol/L NaOH（pH 9.62）為運行緩沖溶液，5%（V/V）甲醇和14 mmol/L的十二烷基磺酸鈉（SDS）為添加劑，分離電壓22 kV，檢測波長250 nm，進樣時間5 s。在優化條件下，葛根素、大豆苷、3'-甲氧基葛根素、3'-羥基葛根素和4'-甲氧基葛根素5種異黃酮可在14 min內完成分離檢測，各目標組分的峰面積與其濃度之間的線性關系良好。該方法用于葛根及其制劑中5種異黃酮的定量分析，加標回收率范圍為95.6%~104.8%，相對標準偏差不超過4.0%。
關鍵詞：膠束毛細管電泳；異黃酮；葛根；制劑
中圖分類號：O657.7 文獻標識碼：A 文章編號：1000-0720（2023）12-1673-05
Simultaneous separation and determination of five isoflavones in Paeonia Lactiflora Radix and its preparations by micellar capillary electrophoresis
ZHANG Chunli，GUO Ailin，CAO Qiue，LI Fei*
School of Chemical Science and Technology，Yunnan University，Kunming 650091，China）
Abstract：A new method of micellar capillary electrophoresis was developed for the simultaneous separation and detection of puerarin，daidzin，3'-methoxypuerarin，3'-hydroxypuerarin，and 4'-methoxypuerarin. The buffer solution consisted of 40 mmol/L Na2B4O7 and 4 mmol/L NaOH （pH 9.62），with 5%（V/V） methanol and 14 mmol/L sodium dodecyl sulfate （SDS） as additives. The separation voltage was 22 kV，the detection wavelength was 250 nm，and the injection time was 5 s. Under the optimized conditions，five isoflavones could be separated and detected within 14 min，and the linear relationship between the peak area of each target component and its concentration was good. The method was applied to the quantitative analysis of five isoflavones in Pueraria lobata and its preparations. The spiked recoveries ranged from 95.6% to 104.8%，and the relative standard deviation was not more than 4.0%.
Keywords：micellar capillary electrophoresis；isoflavones；Paeonia Lactiflora Radix；preparations
氣相色譜-質譜法檢測葡萄酒中二甲基二碳酸鹽
陳波*，羅潔，萬志剛，易冰清，涂小珂，何純點，靳保輝
（深圳海關食品檢驗檢疫技術中心，深圳 518067）
摘要：建立了氣相色譜-質譜（GC-MS）法檢測葡萄酒中二甲基二碳酸鹽代謝產物碳酸甲乙酯的方法，進而建立了二甲基二碳酸鹽添加量的檢測方法。優化了儀器參數、色譜條件、萃取試劑種類和體積、提取時間等參數。結果表明，方法的線性范圍為0.5~30 mg/L，在紅葡萄酒、甜白葡萄酒、起泡葡萄酒中添加0.5，10.0，30.0 mg/L的碳酸甲乙酯，方法回收率為90.0%~110%，相對標準偏差為3.6%~6.7%，檢出限為0.25 mg/L，定量限為0.5 mg/L。該方法適合于葡萄酒中碳酸甲乙酯以及二甲基二碳酸鹽的檢測。
關鍵詞：葡萄酒；氣相色譜-質譜法；二甲基二碳酸鹽；碳酸甲乙酯
中圖分類號：O657.63 文獻標識碼：A 文章編號：1000-0720（2023）12-1678-05
Determination of dimethyldicarbonate in wine by gas chromatography-mass spectrometry
CHEN Bo*，LUO Jie，WAN Zhigang，YI Bingqing，TU Xiaoke，HE Chundian，JIN Baohui
Food Inspection Center of Shenzhen Custom，Shenzhen 518067，China）
Abstract：A method for the determination of methyl ethyl carbonate a metabolite of dimethyl decarbonate in wine by gas chromatography-mass spectrometry （GC-MS） was developed，and then a method for the determination of the added amount of dimethyldecarbonate was established. The analytical equipment parameters，chromatographic conditions，type and volume of extraction reagents，and extraction time were optimized. The linear range of this method was 0.5-30 mg/L. The average recoveries for methyl ethyl carbonate spiked at 0.5，10.0 and 30.0 mg/L in red wine，sweet white wine and sparkling wine ranged from 90.0% to 110%，the relative standard deviations were 3.6%-6.7%，the limit of detection was 0.25 mg/L，and the limit of quantification was 0.5 mg/L. The method is suitable for the detection of methyl ethyl carbonate and dimethyl dicarbonate in wine.
Keywords：wine；gas chromatography-mass spectrometry；dimethyl decarbonate；methyl ethyl carbonate
電感耦合等離子體發射光譜法同時測定鐠釹氧化物中氯和硫含量
趙艷，謝艷艷*，白曉艷*，高燕，付娜，陳雄飛，胡夢橋，張力久
（國標（北京）檢驗認證有限公司，北京 100088）
摘要：建立了一種電感耦合等離子體發射光譜（ICP-OES）同時測定鐠釹氧化物中氯（Cl）和硫（以SO42-形式存在）含量的方法。讀取真空紫外波段129~190 nm譜線信號，優化了測試參數。使用硝酸低溫溶解樣品，選擇分析譜線為Cl（134.724 nm）和S（180.731 nm），標準曲線法測定。在優化條件下，Cl和S在0~10 mg/L范圍內線性相關系數均為0.9999，Cl回收率為93.1%~107.2%，相對標準偏差（RSD）為4.8%；S回收率為89.9%~94.9%，RSD為3.8%。該方法可以檢測鐠釹氧化物材料中含量大于0.014%的Cl和含量大于0.003%的S。
關鍵詞：電感耦合等離子體發射光譜；鐠釹氧化物；氯和硫
中圖分類號：O657.31 文獻標識碼：Ａ 文章編號：1000-0720（2023）12-1683-06
Simultaneous determination of chlorinity and sulfur in praseodymium neodymium oxides by inductively coupled plasma optical emission spectroscopy
ZHAO Yan，XIE Yanyan*，BAI Xiaoyan*，GAO Yan，FU Na，CHEN Xiongfei，HU Mengqiao，ZHANG Lijiu
Guobiao （Beijing） Testing & Certification Co.，Ltd.，Beijing 100088，China）
Abstract：A method for the determination of the chlorinity （Cl） and sulfur （existing as SO42-） contents in praseodymium neodymium oxides by inductively coupled plasma optical emission spectroscopy （ICP-OES） was established. Spectral line signals of 129-190 nm in the vacuum ultraviolet band were recorded and the instrument parameters were optimized. The sample was fully dissolved using nitric acid at low temperatures. Under the optimized conditions，the spectral lines selected for analysis were Cl （134.724 nm） and S （180.731 nm）. There were good linear relationships for Cl and S，with the correlation coefficients （r） of 0.9999. The standard addition recoveries were 93.1%-107.2% for Cl and 89.9%-94.9% for S，the relative standard deviations （RSDs） were 4.8% for Cl and 3.8% for S. This method could be used to determine Cl content higher than 0.014% and S content higher than 0.003% in praseodymium neodymium oxide materials.
Keywords：ICP-OES；praseodymium neodymium oxides；chlorinity and sulfur
尿樣中低濃度19-去甲基雄酮的來源確證
溫超*，王靜竹，朱天碩，劉欣，王杉
（北京體育大學北京興奮劑檢測實驗室，北京 100029）
摘要：建立了19-去甲基雄酮（19NA）的氣相色譜-燃燒-同位素比質譜（GC/C/IRMS）確證方法，使用高效液相色譜（HPLC）法對尿樣中低濃度的19NA進行分離富集。方法檢出限可達2 ng/mL，回收率為75%，線性范圍為2~15 ng/mL，19NA的測量不確定度為0.76‰。本方法可在24 h內完成19NA的溯源確證，具有高選擇性和檢測效率，可用于興奮劑常規檢測。
關鍵詞：19-去甲基雄酮；興奮劑檢測；高效液相色譜；分離富集
中圖分類號：O657.63；O657.7 文獻標識碼：A 文章編號：1000-0720（2023）12-1689-06
Source confirmation for low concentration of 19-norandrosterone in urine sample
WEN Chao*，WANG Jingzhu，ZHU Tianshuo，LIU Xin，WANG Shan
Beijing Anti-doping Laboratory，Beijing Sport University，Beijing 100029，China）
Abstract：A method based on gas chromatography-combustion-isotope ratio mass spectrometry （CG-C-IRMS） was established for source confirmation of trace amount 19-Norandrosterone （19NA） in human urine. The HPLC was employed for the separation and enrichment of 19NA. The detection limit of 19NA was 2 ng/mL，the method linearity range was 2-15 ng/mL，and the recovery was 75%. Additionally，the measurement uncertainty of 19NA was 0.76‰. The method can complete the traceability confirmation of 19NA within 24 h，with high selectivity and efficiency，and has strong application prospects in procedures for dope testing.
Keywords：19-norandrosterone；anti-doping analysis；HPLC；isolation and enrichment
全固態離子選擇性電極在金屬離子檢測中的應用進展
李懷松1，3，劉海興2，3，張文品*1，4，徐溢*1，2，3
（1. 重慶大學化學化工學院，重慶 400044；2. 重慶大學光電工程學院，重慶 400044；3. 重慶大學新型微納器件與系統技術重點學科實驗室和光電技術與系統教育部重點實驗室，重慶 400044；4. 重慶市特種設備檢測研究院，重慶 401121）
摘要：水環境中金屬離子含量是水質質量的重要指標，研發簡便、靈敏和準確的新型水環境金屬離子檢測技術已成為人們關注的熱點。基于全固態離子選擇電極（ASS-ISE）的電位分析技術，能實現對特定離子的快速電位響應，可滿足在環境監測等領域對金屬離子的實時、快速和原位檢測需求。介紹了ASS-ISE法的原理及分類，綜述了贗電容型、雙電層電容型ASS-ISE及集成ASS-ISE電位傳感器的微流控芯片在金屬離子檢測中的應用進展。
關鍵詞：全固態離子選擇性電極；電位傳感器；金屬離子檢測；微流控芯片
中圖分類號：O657.1 文獻標識碼：A 文章編號：1000-0720（2023）12-1695-10
Application progress of all solid state ion-selective electrodes in metal ion detection
LI Huaisong1，3，LIU Haixing2，3，ZHANG Wenpin*1，4，XU Yi*1，2，3
1. School of Chemistry and Chemical Engineering，Chongqing University，Chongqing 400044，China；2. School of Optoelectronic Engineering，Chongqing University，Chongqing 400044，China；3. Key Disciplines Lab of Novel Micro-Nano Devices and System Technology & Key Laboratory of Optoelectronic Technology and Systems，Ministry of Education，Chongqing University，Chongqing 400044，China；4. Chongqing Special Equipment Inspection and Research Institute，Chongqing 401121，China）
Abstract：The content of metal ion in water environment is an important index of water quality. Much more attention has been paid on the development of simple，sensitive and accurate detecting technology for metal ions in water environment. The potential analytical methods based on all-solid-state ion selective electrode（ASS-ISE） could achieve rapid potential response to specific ions and meet the needs of real-time，rapid and in-situ detection of metal ions in environmental monitoring and other fields. In this paper，the principle and classification of ASS-ISE methods were introduced. The application progress of pseudo-capacitive ASS-ISE and double-layer capacitive ASS-ISE in metal ions detection was reviewed. In particular，microfluidic chip integrated with ASS-ISE potential sensor was concerned in the application of metal ions detection.
Keywords：all solid state ion-selective electrodes （ASS-ISE）；potential sensor；metal ions detection；microfluidic chip
