高效液相色谱-串联质谱法测定猪可食性组织中烯丙孕素残留  

Determination of altrenogest residue in pig edible tissue by a high performance liquid chromatography-tandem mass spectrometry method

作　　者：倪香艳 孙念霞 于寒冰 方芳 孙志文 NI Xiang-yan;SUN Nian-xia;YU Han-bing;FANG Fang;SUN Zhi-wen(Beijing Agricultural Product Quality and Safety Center,Beijing 102629,China;Anhui University of Chinese Medicine,Hefei,Anhui 230012,China)

机构地区：[1]北京市农产品质量安全中心,北京102629 [2]安徽中医药大学,安徽合肥230012

出　　处：《食品与机械》2023年第2期45-49,共5页Food and Machinery

基　　金：安徽省高等学校科学研究项目(编号:KJ2021A0593)。

摘　　要：目的:测定猪可食性组织(肌肉、肝脏、脂肪)中烯丙孕素残留。方法:试样经β-葡萄糖醛酸酶/芳基硫酸酯酶酶解,乙腈提取,PRiME HLB固相萃取柱净化。以乙腈-0.1%甲酸水溶液作为流动相,经Waters UPLC BEH C_(18)反相色谱柱分离后于电喷雾正离子模式下检测,基质匹配外标法定量。结果:烯丙孕素在1~50μg/L的质量浓度范围内线性良好,线性相关系数R^(2)>0.99;该方法在猪肌肉、肝脏、脂肪组织中检测限为0.5μg/kg,定量限为1.0μg/kg。在3个添加水平下(1.0,2.0,10.0μg/kg),平均回收率为60.9%~89.8%,日内变异系数为0.8%~7.1%,日间变异系数为2.5%~11.6%。结论:该方法操作简便,适用于猪可食性组织中烯丙孕素残留的定性与定量分析。Objective:To determinate the residues of altrenogest in porcine edible tissues(muscle,liver,fat),a high performance liquid chromatography-tandem mass spectrometry(LC-MS/MS)method was established.Methods:The samples were hydrolyzed withβ-glucuronidase/arylsulfase,extracted by acetonitrile(ACN),purified by PRiME HLB solid phase extraction column.LC separation was performed with Waters UPLC BEH C_(18) reversed-phase chromatography with a linear gradient elution of acetonitrile(ACN)-0.1%formic acid(FA)as the mobile phase.The samples were detected by electrospray in positive ion mode.Results:The pregnancin in tissues were quantified in the range of 1~50μg/L with good linearity and high linear correlation coefficient(R^(2)>0.99).The limit of detection(LOD,S/N=3)and the limit of quantification(LOQ,S/N=10)were as low as 0.5μg/kg and 1.0μg/kg separately.Under three different concentrations(1.0,2.0,10.0μg/kg),the average recoveries were 60.9%~89.8%,the intra-day coefficient of variation was 0.8%~7.1%,and the inter-day coefficient of variation was 2.5%~11.6%.Conclusion:The method is simple and suitable for the qualitative and quantitative analysis of altrenogest residue in porcine edible tissues.

关 键 词：高效液相色谱-串联质谱法 猪肌肉 猪肝脏 猪脂肪 烯丙孕素 残留检测 

分 类 号：O657.63[理学—分析化学] TS207.3[理学—化学]