QuEChERS净化-高效液相色谱-串联质谱法测定蜂蜜中农药及抗生素的含量
Determination of Pesticides and Antibiotics in Honey by QuEChERS-HPLC-MS/MS
摘 要
样品经pH 4.0的Na2EDTA-Mcllvaine缓冲溶液稀释后，用乙酸-乙腈（1+19）混合溶液提取样品中农药及抗生素后，提取液中加入盐析剂分层，上清液放入盛有磁性C18和N-丙基乙二胺吸附剂的净化瓶中净化，采用Luna C18色谱柱，以不同体积比的0.1%（体积分数）甲酸溶液和乙腈组成的混合液为流动相进行梯度洗脱。以电喷雾正离子源和多反应监测模式进行质谱分析。30种化合物的质量分数在一定范围内与峰面积呈线性关系，检出限（3S/N）在0.3~4.1 μg·kg-1之间。按标准加入法进行回收试验，回收率在71.1%~116%之间，测定值的相对标准偏差（n=5）在0.80%~21%之间。
QuEChERS
蜂蜜
农药
兽药
HPLC-MS/MS
QuEChERS
honey
pesticide
antibiotic
Abstract
The sample was diluted with pH 4.0 of Na2EDTA-Mcllvaine buffer solution, and pesticides and antibiotics in the sample were extracted with a mixture of acetic acid-acetonitrile (1+19), and the extract was stratified by salting-out agents. The supernatant was cleaned up with purification pipe filled with magnetic C18 and PSA. Luna C18 column was used as stationary phase, and a mixture of 0.1% (φ) formic acid solution and acetonitrile in various ratios as mobile phase in gradient elution. ESI+ and MRM were adopted in MS. Linear relationships between values of peak area and mass concentration of 30 compounds were found in definite ranges, with detection limits (3S/N) in the range of 0.3-4.1 μg·kg-1. Test for recovery was made by standard addition method, giving results in the range of 71.1%-116%, with RSDs (n=5) ranged from 0.80% to 21%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201707001
所属栏目 试验与研究
基金项目 浙江省自然科学基金项目（LY16B050008）；浙江省科技厅公益项目（2015C32006）；农业部农药残留检测重点实验室资助项目（2014PRG01）；杭州市钱江特聘专家项目（2014）
收稿日期 2016/6/1
修改稿日期
网络出版日期
作者单位点击查看
联系人作者李祖光(lzg@zjut.edu.cn)
备注苗琼晨(1990-),女,河南新乡人,硕士研究生,研究方向为仪器分析和样品前处理技术
引用该论文: MIAO Qiongchen,NIE Jing,WU Huizhen,QIAN Mingrong,SUN Caixia,LI Zuguang. Determination of Pesticides and Antibiotics in Honey by QuEChERS-HPLC-MS/MS[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2017, 53(7): 745～752
苗琼晨,聂晶,吴慧珍,钱鸣蓉,孙彩霞,李祖光. QuEChERS净化-高效液相色谱-串联质谱法测定蜂蜜中农药及抗生素的含量[J]. 理化检验－化学分册, 2017, 53(7): 745～752
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参考文献
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【2】张桂凤,游勇基.蜂产品中四环素类药物残留检测方法研究进展[J].海峡药学, 2010,22(8):4-7.
【3】徐书法,曹坦,辛广,等.蜂产品中抗生素残留检测技术研究概况[J].现代科学仪器, 2009(4):134-140.
【4】李岩,邵兵,徐锁洪.动物性食品内大环内酯类抗生素残留分析[J].中国卫生检验杂志, 2005,15(10):1275-1277.
【5】BLASCO C, PICO Y, TORRES C M, et al. Progress in analysis of residual antibacterials in food[J]. TrAC Trends in Analytical Chemistry, 2007,26(9):895-913.
【6】李周敏,邵诚,方惠群.蜂蜜中残留抗生素的检测方法研究[J].安徽医药, 2012,16(5):568-570.
【7】KMELLAR B, ABRANKO L, FODOR P, et al. Routine approach to qualitatively screening 300 pesticides and quantification of those frequently detected in fruit and vegetables using liquid chromatography tandem mass spectrometry (LC-MS/MS)[J]. Food Additives and Contaminants:Part A, 2010,27(10):1415-1430.
【8】FARAJZADEH M A, MOGADDAM M R A, GHORBANPOUR H. Development of a new microextraction method based on elevated temperature dispersive liquid-liquid microextraction for determination of triazole pesticides residues in honey by gas chromatography-nitrogen phosphorus detection[J]. Journal of Chromatography A, 2014,1347:8-16.
【9】LIU H Y, LIN S L, FUH M R. Determination of chloramphenicol, thiamphenicol and florfenicol in milk and honey using modified QuEChERS extraction coupled with polymeric monolith-based capillary liquid chromatography tandem mass spectrometry[J]. Talanta, 2016,150:233-239.
【10】SHENDY A H, AL-GHOBASHY M A, MOHAMMED M N, et al. Simultaneous determination of 200 pesticide residues in honey using gas chromatography-tandem mass spectrometry in conjunction with streamlined quantification approach[J]. Journal of Chromatography A, 2015,1427:142-160.
【11】WANG J, LEUNG D. The challenges of developing a generic extraction procedure to analyze multi-class veterinary drug residues in milk and honey using ultra-high pressure liquid chromatography quadrupole time-of-flight mass spectrometry[J]. Drug Testing and Analysis, 2012,4(s1):103-111.
【12】LOMBARDO-AGUI M, GARCLA-CAMPAÑA A M, GAMIZ-GARCIA L, et al. Determination of quinolones of veterinary use in bee products by ultra-high performance liquid chromatography-tandem mass spectrometry using a QuEChERS extraction procedure[J]. Talanta, 2012,93:193-199.
【13】ZHANG Y Q, LIU X M, LI X, et al. Rapid screening and quantification of multi-class multi-residue veterinary drugs in royal jelly by ultra performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry[J]. Food Control, 2016,60:667-676.
【14】LI S S, LIU X G, DONG F S, et al. Chemometric-assisted QuEChERS extraction method for the residual analysis of thiacloprid, spirotetramat and spirotetramat's four metabolites in pepper:Application of their dissipation patterns[J]. Food Chemistry, 2016,192:893-899.
【15】王伟,石志红,康健,等.改进的QuEChERS结合LC-MS/MS同时测定蜂蜜中60种兽药残留[J].分析实验室, 2013,32(4):82-88.
【16】KUJAWSKI M W, NAMIESNIK J. Challenges in preparing honey samples for chromatographic determination of contaminants and trace residues[J]. TrAC Trends in Analytical Chemistry, 2008,27(9):785-793.
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