高效液相色谱-串联质谱法同时测定动物源性食品中35种兽药残留量
Simultaneous HPLC-MS/MS Determination of 35 Veterinary Drugs in Animal Derived Food
摘 要
提出了高效液相色谱-串联质谱法同时测定动物源性食品中35种兽药残留量的方法。样品经含1%(体积分数)乙酸的乙腈提取,QuEChERS方法净化,所得净化液以Zobax Eclipse Plus C18色谱柱为分离柱,以不同体积比的0.1%甲酸(体积分数)溶液和乙腈混合液为流动相进行梯度洗脱,采用电喷雾正离子源和多反应监测模式检测。35种化合物的质量分数均在1~50 μg·kg-1范围内与其峰面积呈线性关系,方法的检出限(3S/N)在0.02~1.07 μg·kg-1之间,测定下限(10S/N)在0.08~3.58 μg·kg-1之间。以空白样品为基体进行加标回收试验,所得回收率在45.6%~121%之间,相对标准偏差(n=6)在2.4%~24%之间。
兽药
动物源性食品
HPLC-MS/MS
Veterinary drugs
Food of animal origin
Abstract
A method of HPLC-MS/MS for the simultaneous determination of 35 veterinary drugs in food of animal origin was proposed. The sample was extracted with acetonitrile (containing 1% by vol. of acetic acid) and purified by the QuEChERS method. Zobax Eclipse Plus C18 column was used as stationary phase in chromatographic separation, and the mixture of 0.1% (φ) formic acid solution and acetonitrile mixed in different ratio was used as mobile phase in gradient elution. ESI+ and multi-reaction monitoring were adopted in MS/MS. Linear relationships between values of peak area and mass fraction of the 35 compounds were kept in the same range of 1-50 μg·kg-1, with detection limits (3S/N) in the range of 0.02-1.07 μg·kg-1 and lower limits of determination (10S/N) in the range of 0.08-3.58 μg·kg-1. On the base of blank sample, test for recovery was made by standard addition method; values of recovery found were in the range of 45.6%-121%, with RSD′s (n=6) in the range of 2.4%-24%.
中图分类号 O657.63
所属栏目 试验与研究
基金项目 上海市技术性贸易壁垒专项(12DZ0503102)
收稿日期 2013/5/16
修改稿日期
网络出版日期
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备注陈刚(1988-),男,上海人,硕士研究生,主要研究方向为食品安全与检测。
引用该论文: CHEN Gang,DENG Xiao-jun,SUN Jin-lan,LI Jian-zhong,CHEN Shun-sheng,SONG Qing,ZHAO Shan-zhen. Simultaneous HPLC-MS/MS Determination of 35 Veterinary Drugs in Animal Derived Food[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2014, 50(7): 809～814
陈刚,邓晓军,孙锦兰,李建中,陈舜胜,宋青,赵善贞. 高效液相色谱-串联质谱法同时测定动物源性食品中35种兽药残留量[J]. 理化检验－化学分册, 2014, 50(7): 809～814
被引情况:
【1】庾金良,张晓燕,卜洪忠,丁涛,沈崇钰,吴斌,陈慧兰,殷耀,陈磊,吕辰, "高效液相色谱-串联质谱法测定鸡肉产品中金刚烷胺残留量",理化检验－化学分册 51, 224-227(2015)
【2】张晓强,张波,方萍,林慧,颜春荣, "QuEChERS-超高效液相色谱-串联质谱法快速测定鱼肉中22种磺胺类药物残留",理化检验－化学分册 51, 369-374(2015)
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参考文献
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【11】卢大胜,熊丽蓓,温忆敏,等.QuEChERS前处理方法联合GPC-GC/MS在测定蔬菜水果农药残留中的应用［J］.质谱学报, 2011,32(4):229-235.
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【15】JEMMA K, MICHELLE W, MARTIN D, et al. Benzimidazole carbamate residues in milk: detection by surface plasmon resonance-biosensor, using a modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method for extraction［J］. Analytica Chimica Acta, 2009,654:111-119.
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【2】李晓丽,李娜,李鹏,等.高分子印记固相萃取-液相色谱-质谱法测定水产品中孔雀石绿、结晶紫、亮绿及其代谢产物［J］.中国食品卫生杂志, 2012,24(3):209-214.
【3】李艳霞,李帷.固相萃取-高效液相色谱法同时检测畜禽粪便中14种兽药抗生素［J］.分析化学, 2012,40(2):213-217.
【4】郭德华,邓晓军,赵善贞,等.固相萃取-高效液相色谱/串联质谱同时检测动物源性食品中76种兽药残留［J］.分析化学, 2010,38(3):318-324.
【5】林维宣,董伟峰,陈溪,等.气相色谱-质谱法同时检测动物组织中多种激素类兽药的残留量［J］.色谱, 2009,27(3):294-298.
【6】卜明楠,石志红,康健,等.QuEChERS结合LC-MS/MS同时测定虾肉中72种兽药残留［J］.分析测试学报, 2012,31(5):552-558.
【7】GEORGE S, TIMOTHY B. The development and validation of a multiclass liquid chromatography tandem mass spectrometry (LC-MS/MS) procedure for the determination of veterinary drug residues in animal tissue using a QuEChERS (QUick, Easy, CHeap, Effective,Rugged and Safe) approach［J］. Analytica Chimica Acta, 2009,637:68-78.
【8】XU Rong, WU Jian-wei, LIU You-gang, et al. Analysis of pesticide residues using the Quick Easy Cheap Effective Rugged and Safe (QuEChERS) pesticide multiresidue method in traditional Chinese medicine by gas chromatography with electron capture detection［J］. Chemosphere, 2011,84:908-912.
【9】LEHOTAY S J, MASTOVSKA K, YUN S J. Evaluation of two fast and easy methods for pesticide residue analysis in fatty food matrixes［J］. Journal of AOAC International, 2005,88:630-633.
【10】黄超群,丁慧瑛,朱晓雨,等.液相色谱-串联质谱法同时测定蔬菜中7种三唑醇类杀菌剂的残留量［J］.分析测试学报, 2011,30(6):656-660.
【11】卢大胜,熊丽蓓,温忆敏,等.QuEChERS前处理方法联合GPC-GC/MS在测定蔬菜水果农药残留中的应用［J］.质谱学报, 2011,32(4):229-235.
【12】URAIRAT K, LEHOTAY S J, MIAO S, et al. High throughput analysis of 150 pesticides in fruits and vegetables using QuEChERS and low-pressure gas chromatography-time-of-flight mass spectrometry［J］. Journal of Chromatography A, 2010,1217:6692-6703.
【13】EWA C, ANNA S R, JUAN M M R, et al. Evaluation of QuEChERS method for the determination of organochlorine pesticide residues in selected groups of fruits［J］. Food Chemistry, 2011,125:773-778.
【14】郭俊峰,马昕,尚楠.液相色谱-质谱/质谱法快速测定牛奶中的氯舒隆残留量［J］.食品科学, 2008,29(12):638-640.
【15】JEMMA K, MICHELLE W, MARTIN D, et al. Benzimidazole carbamate residues in milk: detection by surface plasmon resonance-biosensor, using a modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method for extraction［J］. Analytica Chimica Acta, 2009,654:111-119.
【16】ANGELIKA W, MAREK B. Determination of pesticide residues in food matrices using the QuEChERS methodology［J］. Food Chemistry, 2011,125:803-812.
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