摘要
目的建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)测定水产品及其制品中3种抗生素和14种性激素残留量的分析方法。方法样品经乙酸乙酯提取,GCB/NH2固相萃取小柱净化,洗脱液氮气吹至近干,用甲醇-水(1:9,V:V)溶液溶解,采用大气压电离离子(atmospheric pressure chemical ionization,APCI)源,正负离子模式采集,多反应监测方式(multiple reaction monitoring, MRM)检测,基质匹配外标法,定性和定量分析氯霉素、甲砜霉素、氟甲砜霉素、丙酸睾酮、睾丸酮、甲基睾丸酮、雌酮、雌二醇、雌三醇、己烯雌酚、醋酸甲地孕酮、炔诺酮、醋酸氯地孕酮、诺龙、康力龙、苯丙酸诺龙、群勃龙的残留量。结果 17种激素在2～200μg/L范围内线性兲系良好,相兲系数均大于0.99,定量限为1.5～3μg/kg;添加水平为5～15μg/kg,平均回收率在65%～100%,相对标准偏差为1%～9%。结论该方法简单、快捷,可作为水产品及其制品中17种激素的检测方法。
Objective To establish a method for the determination of 3 antibiotics and 14 sex hormones in aquatic products and their products by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Methods The sample was extracted with ethyl acetate,purified by GCB/NH2 solid phase extraction column,and the eluent which got from above conditions was dried nearly by nitrogen-blow,and dissolved in methanol-water solution(1:9,V:V),Finally,they were ionized by atmospheric pressure chemical ion(APCI)source,collected in positive and negative ion mode,and matrix matched with external standard method.The qualitative and quantitative determination for the thiamphenicol,fluorothiamphenicol,testosterone propionate,testosterone,methyltestosterone,estrone,estradiol,estriol,diethylstilbestrol,medroxyprogesterone acetate,norethisterone,chlormadinone acetate,norolone,conlon,phenylpropanolone,and trenbolone were detected by UPLC-MS/MS in multiple reaction monitoring(MRM)mode.Results The results showed that 17 kinds of hormones had good linear relationships in the range of 2-200μg/L with correlation coefficients better than 0.99.The limits of quantitation were 1.5-3μg/kg.The average recoveries of the method ranged from 65%to 100%at the spiked levels of 5-15μg/kg for the 17 hormones,with the relative standard deviations(RSDs)of 1%-9%.Conclusion This method is simple and quick,which can be used as the detection method of 17 hormones in aquatic products and their products.
作者
杨帆
莫文电
段玉林
韦志疆
黄兴振
容秀湾
覃振真
秦峰
陈桂良
YANG Fan;MO Wen-Dian;Duan Yu-Lin;WEI Zhi-Jiang;HUANG Xing-Zhen;RONG Xiu-Wan;QIN Zhen-Zhen;QIN Feng;CHEN Gui-Liang(Guangxi Hechi Institute for Food and Drug Control,Hechi 547000,China;Guangxi Food and Drug Evaluation and Verification Center,Nanning 530022,China;College of Pharmacy,Guangxi Medical University,Nanning 530022,China;Shanghai Institute for Food and Drug Control,Shanghai 201203,China;Shanghai Drug Evaluation and Verification Center,Shanghai 201203,China)
出处
《食品安全质量检测学报》
CAS
2019年第8期2247-2257,共11页
Journal of Food Safety and Quality
基金
2017年国家食品药品监督管理总局食品补充检验方法项目~~
关键词
大气压电离离子源
超高效液相色谱-串联质谱法
抗生素
性激素
水产品及其制品
atmospheric pressure chemical ionization ion source
ultra performance liquid chromatography-tandem mass spectrometry
antibiotics
sex hormone
aquatic products and their products
作者简介
通讯作者:莫文电,副主仸药师,主要研究方向为食品、药品、化妆品安全检测。E-mail:279396103@qq.com;杨帆,主管药师,主要研究方向为食品、药品和化妆品检验检测。E-mail:410389865@qq.com
