超高效液相色谱-串联质谱法测定畜产品中6种青霉素类药物残留
Determination of 6 Penicillin Residues in Livestock Products by UHPLC-MS/MS
摘 要
采用超高效液相色谱-串联质谱法快速测定牛肉和牛奶中青霉素类药物残留.样品以磷酸盐缓冲溶液提取、乙酸锌沉淀蛋白、正己烷脱脂,然后经HLB固相萃取柱净化后,采用超高效液相色谱-串联质谱分离检测,外标法定量.6种青霉素的线性范围均在25.0 μg·L-1以内,检出限(3S/N)为2 μg·kg-1,测定下限(10S/N)为5 μg·kg-1.加标回收率在77.0%~99.8%之间,测定值的相对标准偏差(n=6)在3.7%~13%之间.
青霉素
畜产品
UHPLC-MS/MS
Penicillin
Livestock products
Abstract
A UHPLC-MS/MS method was used to measure penicillin residues in beef and milk. The sample was extracted with NaH2PO4 solution. Zinc acetate was used to precipitate proteins,and hexane was used for defatting. The extract was then purified on a HLB solid phase extraction column. The penicillin was detected by UHPLC-MS/MS and quantified by external standard method. The linear ranges of 6 kinds of penicillin were within 25.0 μg·L-1,the detection limit (3S/N) was 2 μg·kg-1 and the lower limit of determination (10S/N) was 5 μg·kg-1. The recovery rates measured by standard addition method were in the range of 77.0%-99.8%,with RSD (n=6) was in the range of 3.7%-13%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201506006
所属栏目 工作简报
基金项目 天津检验检疫局科技计划项目(TK076-2013)
收稿日期 2014/5/22
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备注王飞(1986-),女,河北石家庄人,助理工程师,硕士,主要研究方向为农兽药及食品添加剂检测.
引用该论文: WANG Fei,CHEN Qi-yong,MI Jie-bo,CHAI Jia. Determination of 6 Penicillin Residues in Livestock Products by UHPLC-MS/MS[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2015, 51(6): 756～760
王飞,陈其勇,宓捷波,柴佳. 超高效液相色谱-串联质谱法测定畜产品中6种青霉素类药物残留[J]. 理化检验－化学分册, 2015, 51(6): 756～760
被引情况:
【1】姜凤丽,滕小梅,倪春芳,梁 晨,汪 蓉,曾立波,张玉荣, "超高效液相色谱-串联四极杆飞行时间质谱法筛查人全血中150种药物与毒物",理化检验－化学分册 52, 417-426(2016)
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参考文献
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【11】李学民,母健,王蕾,等.液相色谱-串联质谱法测定蜂蜜中9种青霉素[J].河北大学学报,2012,32(5):492-498．
【12】KANG S Y,PARK S,KIM M J,et al. A sensitive and selective LC-MS/MS analysis coupled with an online sample enrichment technique for H295R steroidogenesis assay and its application in the investigation of the effect of sildenafil on steroidogenesis[J]. Analytical and Bioanalytical Chemistry,2013,405(29):9489-9496．
【13】TYCZKOWSKA K L. Solvent degradation of cloxacillin in vitro: Tentative identification of degradation products using thermospray liquid chromatography-mass spectrometry[J]. Journal of Chromatography A,1992,594(1/2):195-201．
【14】WIESE B,MARTIN K. Basic extraction studies of benzylpenicillin and its determination by liquid chromatography with pre-column derivatisation[J]. Journal of Pharmaceutical and Biomedical Analysis,1989,7(1):67-78．
【15】GB/T 20755-2006畜禽肉中九种青霉素类药物残留量的测定液相色谱-串联质谱法[S].
【2】GAUDINA V,MARISA P,FUSELIERA R,et al. Validation of a microbiological method: the STAR protocol,a five-plate test,for the screening of antibiotic residues in milk[J]. Food Additives and Contaminants,2004,21(5):422-433．
【3】FOSTER J W,WOODRUFF H B. Microbiological aspects of penicillin I.[J]. Journal of Bacteriology,1943,46(2):187-202．
【4】PETZ M. Recent applications of surface plasmon resonance biosensors for analyzing residues and contaminants in food[J]. Monatshefte für Chemie - Chemical Monthly,2009,140(8):953-964．
【5】VORC L,SOCHR J,RIEVAJ M,et al. Voltammetric determination of penicillin V in pharmaceutical for -mulations andhumanurineusing aboron-doped amond electrode[J]. Bioelectrochemistry,2012,88:36-41．
【6】SARTORI E R,VICENTINI F C,FATIBELLO-FILHO O. Indirect determination of sulfite using a polyphenol oxidase biosensor based on a glassy carbon electrode modified with multi-walled carbon nanotubes and gold nanoparticles within a poly(allylamine hydrochloride) film[J]. Talanta,2011,87:235-242．
【7】PENG J,CHENG G Y,HUANG L L,et al. Development of a direct ELISA based on carboxy-terminal of penicillin-binding protein BlaR for the detection of β-lactam antibiotics in foods[J]. Analytical and Bioanalytical Chemistry,2013,405(27):8925-8933．
【8】SAMANIDOUA V F,NISYRIOUA S A,PAPADOYANNISA I N. Residue analysis of penicillins in food products of animal origin by HPLC: a review[J]. Journal of Liquid Chromatography and Related Technologies,2007,30(9/10):1145-1204．
【9】OLSEN M A,CUMMINGS P G,KENNEDY-GAB S. The use of deuterium oxide as a mobile phase for structural elucidation by HPLC/UV/ESI/MS[J]. Analytical Chemistry,2000,72:5070-5078．
【10】陈聪,严慧,沈保华,等.超高效液相色谱-串联质谱法同时测定全血中青霉素G及其主要代谢物[J].色谱,2012,30(5):445-451．
【11】李学民,母健,王蕾,等.液相色谱-串联质谱法测定蜂蜜中9种青霉素[J].河北大学学报,2012,32(5):492-498．
【12】KANG S Y,PARK S,KIM M J,et al. A sensitive and selective LC-MS/MS analysis coupled with an online sample enrichment technique for H295R steroidogenesis assay and its application in the investigation of the effect of sildenafil on steroidogenesis[J]. Analytical and Bioanalytical Chemistry,2013,405(29):9489-9496．
【13】TYCZKOWSKA K L. Solvent degradation of cloxacillin in vitro: Tentative identification of degradation products using thermospray liquid chromatography-mass spectrometry[J]. Journal of Chromatography A,1992,594(1/2):195-201．
【14】WIESE B,MARTIN K. Basic extraction studies of benzylpenicillin and its determination by liquid chromatography with pre-column derivatisation[J]. Journal of Pharmaceutical and Biomedical Analysis,1989,7(1):67-78．
【15】GB/T 20755-2006畜禽肉中九种青霉素类药物残留量的测定液相色谱-串联质谱法[S].
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