超高效液相色谱-串联质谱法测定猪肉和猪肝中烯丙孕素残留  

Determination of altrenogest in swine muscle and liver by ultra performance liquid chromatography-tandem mass spectrometry

作　　者：任玉琴 卜仕金[2,3] 王双 钱鸣蓉[4] REN Yu-Qin;BU Shi -Jin;WANG Shuang;QIAN Ming-Rong(Zhejiang Province Institute of Veterinary Drug and Feedstuff, Hangzhou 311199, China;Veterinary Medicine College, Yangzhou University, Yangzhou 225009, China;Jiangsu Co-innovation Center for Prevention and Control of lmportant Animal Infectious Diseases and Zoonoses, Yangzhou 225009, China;Department of Agriculture Agricultural Products and Gm Product Quality Safety Supervision and Testing Centre （Hangzhou）, Hangzhou 311199, China)

机构地区：[1]浙江省兽药饲料监察所,杭州311199 [2]扬州大学兽医学院,扬州225009 [3]江苏省动物重要疫病与人兽共患病防控协同创新中心,扬州225009 [4]农业部农产品及转基因产品质量安全监督检验测试中心(杭州),杭州310021

出　　处：《食品安全质量检测学报》2018年第9期2118-2123,共6页Journal of Food Safety and Quality

基　　金：江苏高校优势学科建设工程资助项目(PAPD)~~

摘　　要：目的建立猪肉和猪肝中烯丙孕素残留测定的超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)。方法肌肉和肝脏样品,经β-葡萄糖醛酸酶/芳基硫酸酯酶酶解、乙腈提取、乙腈饱和正己烷溶液除脂;经乙酸乙酯溶解后,用10%碳酸钠溶液净化,UPLC-MS/MS测定,外标法定量。结果烯丙孕素在猪肉和猪肝中的检测限为0.5μg/kg,定量限为1.0μg/kg;在1.0、2.0和5.0μg/kg浓度添加的回收率为68.8%~87.6%、日内相对标准偏差(relative standard deviation,RSD)为1.8%~8.9%,日间RSD为1.8%~6.9%。结论该方法操作简便、准确、重现性好,适用于猪肌肉、肝脏中烯丙孕素残留物含量测定。Objective To establish a method for determination of altrenogest residues in swine muscle and liver by ultra performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS）. Methods The liver and muscle samples were hydrolyzed by β-glucosidase/arysulfatase and extracted by acetonitrile, then the extracting solution were degreased with n-hexane. After being dissolved with ethyl acetate, the supernatant was purified by 10% sodium carbonate solution. Finally, altrenogest was analyzed by UPLC-MS/MS, and the external method was used. Results Altrenogest had good linearities in the range of 1-200 ng/mL, and the correlation coefficients （r2） were more than 0.99. The limit of quantification was 1.0 μg/kg, and the limit of detection was 0.5 μg/kg. At 3 spiked levels of 1.0, 2.0 and 5.0 μg/kg, the average recoveries were 68.8%-87.6% for altrenogest, with intra-day relative standard deviations （RSDs） of 1.8%-8.9% and inter-day RSDs of 1.8%-6.9%. Conclusion This method is simple, effective and sensitive, which is suitable for determination of altrenogest in swine muscle and liver.

关 键 词：超高效液相色谱-串联质谱法 烯丙孕素 可食性组织中 残留检测 

分 类 号：O657.63[理学—分析化学] TS251.7[理学—化学]