[1]刘畅.蔬菜中二十种磺胺类抗生素残留的QuEChERS-超高效液相色谱-串联质谱法检测[J].黑龙江农业科学,2018,(06):101-105.[doi:10.11942/j.issn1002-2767.2018.06.0101]
　LIU Chang.Determination of Sulfonamides in Vegetables by QuEChERS-high Performance Liquid Chromatography-tandem Mass Spectrometry[J].HEILONGJIANG AGRICULTURAL SCIENCES,2018,(06):101-105.[doi:10.11942/j.issn1002-2767.2018.06.0101]
点击复制

蔬菜中二十种磺胺类抗生素残留的QuEChERS-超高效液相色谱-串联质谱法检测

《黑龙江农业科学》[ISSN:1002-2767/CN:23-1204/S] 卷: 期数: 2018年06期 页码: 101-105 栏目: 出版日期: 2018-06-10
Title:
Determination of Sulfonamides in Vegetables by QuEChERS-high Performance Liquid Chromatography-tandem Mass Spectrometry
作者:
刘畅
哈尔滨市农产品质量安全检验检测中心，黑龙江 哈尔滨，150070
Author(s):
LIU Chang
Harbin Examing and Inspection Center for Agricultural Products Safety and Quality,Harbin 150070,China
关键词:
QuEChERS; 超高效液相色谱-串联质谱; 蔬菜; 磺胺; 多残留
Keywords:
QuEChERS; high performance liquid chromatography-tandem mass spectrometry; vegetables; sulfonamides; more residuals
DOI:
10.11942/j.issn1002-2767.2018.06.0101
文献标志码:
A
摘要:
建立了QuEChERS结合超高效液相色谱-串联质谱仪检测不同种蔬菜中20种磺胺类兽药多残留的检测方法。称取10.0 g样品，以1.0%乙酸乙腈10 mL为提取剂，6 g硫酸镁、1.5 g醋酸钠为萃取盐，使用液-液萃取静置分层，取8 mL上清液经150 mg乙二胺-N-丙基硅烷（PSA）和 900 mg无水硫酸镁净化。再提取净化后的溶液5 mL，在40 ℃下用氮吹仪浓缩，残渣用200 μL乙腈，800 μL水溶解。超高效液相色谱-串联质谱仪采用正离子多反应监测模式，内标法定量。结果表明：在0.5~100 μg/L范围内，20种磺胺类兽药线性良好，相关系数均大于0.99，3个不同添加浓度的回收率在67.4%~116.6% 范围内，相对标准偏差在0.1%~12.8% 范围内，均可满足定量分析要求，该方法操作简单快速，适用于大批量蔬菜样品同时检测兽药多残留。
Abstract:
The methods of detection of 20 sulfonamides in different kinds of vegetables were established by improved QuEChERS combining the ultra-high performance liquid chromatography-tandem mass spectrometer.Samples weight in 10.0 g were extracted by 10 mL 1.0% acetic acid in acetonitrile,6 g magnesium sulfate and 1.5 g sodium acetate and liquid-liquid extraction was used to stand stratification.8 mL supernatant fluid were purified by 150 mg ethylenediamine -N- propyl silane (PSA) and 900 mg magnesium sulfate.Then 5 mL supernatant fluid were concentrated under 40℃ with blowing nitrogen.The residues were dissolved by 200 mL acetonitrile and 800 mL water.The positive ion multi-reaction monitoring mode was used by the super high performance liquid chromatography-tandem mass spectrometer and quantify was used by the internal standard method.The results showed that the range of 0.5-100 μg?L-1,20 sulfonamides were in good linear and the correlation coefficients were greater than 0.99.Three different recovery were between 67.4 and 116.6,standard of standard deviation were between 0.1 and 12.8,all of these were met the requirements of quantitative analysis,and the method was simply rapidly and was suitable for large quantities of vegetables samples at the same time to test veterinary drug residues.

参考文献/References:

［1］Economou V,Gousia P.Agriculture and food animals as a source of antimicrobial-resistant bacteria[J].Infect Drug Resist,2015,8(4):49-61.

[2]Danezis G P,Anagnostopoulos C J,Liapis K,et al.Multi-residue analysis of pesticides,plant hormones,veterinary drugs and mycotoxins using HILIC chromatography-MS/MS in various food matrices[J].Analytica Chimica Acta,2016,942(10):121-138.
[3]Chen H R,Rairat T,Loh S H,et al.Assessment of veterinary drugs in plants using pharmacokinetic approaches: The absorption,distribution and elimination of tetracycline and sulfamethoxazole in ephemeral vegetables[J].PLoS One,2017,12(8):1-16.
[4]Ahmed M B,Rajapaksha A U,Lim J E,et al.Distribution and accumulative pattern of tetracyclines and sulfonamides in edible vegetables of cucumber,tomato,and lettuce[J].Journal of agricultural and food chemistry,2015,63(2):398-405.
[5]张律,岳亚军,赖少阳,等.高效液相色谱-串联质谱法测定生活饮用水中11种抗生素[J].食品安全质量检测学报,2017，8(6):2204-2210.
[6]周爱霞,苏小四,高松,等.高效液相色谱测定地下水、土壤及粪便中4种磺胺类抗生素[J].分析化学,2014，42(3):397-402.
[7]吴晓莲,包艳萍,向垒,等.固相萃取-高效液相色谱-串联质谱法同时测定蔬菜中8种磺胺类抗生素[J].环境化学,2013,32(6):1038-1044.
[8]吴岩,姜冰,徐义刚,等.QuEChERS-液相色谱-串联质谱法同时测定果蔬中16种农药残留[J].色谱,2015，33(3):228-234.
[9]林涛,邵金良,刘兴勇,等.QuEChERS-超高效液相色谱-串联质谱法测定蔬菜中41种农药残留[J].色谱,2015，33(3):235-241.
[10]王飞,宓捷波,李淑静,等.改良的QuEChERS样本前处理/高效液相色谱-串联质谱法检测猪肉中四环素类兽药的残留[J].分析测试学报,2017,36(2):272-275.
[11]X Li,H Yu,R Peng,et al.Determination of 19 sulfonamides residues in pork samples by combining QuEChERS with dispersive liquid-liquid microextraction followed by UHPLC-MS/MS[J].Journal of Separation Science,2017，40(6):1377-1384.
[12]张科明,梁飞燕,邓鸣,等.QuEChERS结合液相色谱-串联质谱法快速测定猪肉中多类兽药残留[J].色谱,2016,34(9):860-867.
[13]熊春兰,郭平,占春瑞,等.高效液相色谱-串联质谱法同时测定水产品中8类38种兽药残留[J].分析测试学报,2013,32(2):193-198.
[14]胡文彦,许磊,杨军,等.基于QuEChERS提取的快速液相色谱-串联质谱法测定婴幼儿谷基辅助食品中的9种真菌毒素[J].色谱,2014,32(2):133-138.

相似文献/References:

[1]张海霞,徐晶,徐连伟,等.利用QuEChERS法筛查并分析哈尔滨市“地趴”储玉米中的真菌毒素[J].黑龙江农业科学,2017,(08):73.[doi:10.11942/j.issn1002-2767.2017.08.0073]
　ZHANG Hai-xia,XU Jing,XU Lian-wei,et al.Screening and Analysis of the Mycotoxin in the Maize Stored on the Ground of Harbin by QuEChERS Method[J].HEILONGJIANG AGRICULTURAL SCIENCES,2017,(06):73.[doi:10.11942/j.issn1002-2767.2017.08.0073]
[2]张海霞,杨静,刘畅,等.QuEChERS-超高效液相色谱-串联质谱法快速检测玉米中7种真菌毒素[J].黑龙江农业科学,2017,(07):61.[doi:10.11942/j.issn1002-2767.2017.07.0061]
　ZHANG Hai-xia,YANG Jing,LIU Chang,et al.Rapid Detection of Seven Mycotoxins in Maize by QuEChERS with Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry[J].HEILONGJIANG AGRICULTURAL SCIENCES,2017,(06):61.[doi:10.11942/j.issn1002-2767.2017.07.0061]
[3]姜涛,赵琳,兰静,等.QuEChERS-超高效液相色谱串联质谱法测定玉米中的17种真菌毒素[J].黑龙江农业科学,2019,(11):106.[doi:10.11942/j.issn1002-2767.2019.11.0106]
　JIANG Tao,ZHAO Lin,LAN Jing,et al.Determination of 17 Mycotoxins in Maize by QuEChERS-ultra High Performance Liquid Chromatography Tandem Mass Spectrometry[J].HEILONGJIANG AGRICULTURAL SCIENCES,2019,(06):106.[doi:10.11942/j.issn1002-2767.2019.11.0106]

备注/Memo

收稿日期：2018-03-06作者简介：刘畅（1988-）,女，硕士，农艺师，从事药残检测研究。E-mail:y150030@126.com。

更新日期/Last Update: 2018-09-12