超高效液相色谱-串联质谱法测定水产品及其制品中3种抗生素和14种性激素残留量
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2~200 μg/L范围内线性关系良好, 相关系数均大于0.99, 定量限为1.5~3 μg/kg; 添加水平为5~15 μg/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?200 μg/L with correlation coefficients better than 0.99. The limits of quantitation were 1.5?3 μg/kg. The average recoveries of the method ranged from 65% to 100% at the spiked levels of 5?15 μg/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.
标题：超高效液相色谱-串联质谱法测定水产品及其制品中3种抗生素和14种性激素残留量
英文标题：Determination of residues of 3 antibiotics and 14 sex hormones in aquatic products and their products by ultra performance liquid chromatography-tandem mass spectrometry
作者：
杨帆 广西河池食品药品检验所
莫文电 广西河池食品药品检验所
段玉林 广西食品药品审评查验中心
黄兴振 广西医科大学药学院
韦志疆 广西河池食品药品检验所
容秀湾 广西河池食品药品检验所
覃振真 广西河池食品药品检验所
秦峰 上海市食品药品检验所
陈桂良 上海药品审评核查中心
中文关键词: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,
英文关键词:atmospheric pressure chemical ionization ion source,ultra performance liquid chromatography-tandem mass spectrometry,antibiotics,sex hormone,aquatic products and their products,
发表日期：2019-01-24
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