摘要
采用分散固相萃取的前处理技术,建立了一种UPLC-MS/MS法测定梅花鹿鹿茸中醋酸氯地孕酮的检测方法。鹿茸样品以乙腈为提取剂,经50 mg PSA净化。液相色谱条件:ACQUITY BEH C18柱(2.1 mm×50 mm,1.7μm),流动相A为乙腈,流动相B为水,柱温35℃;质谱条件:正离子模式(ESI+),多反应监测(MRM)模式。鹿茸中醋酸氯地孕酮含量采用外标法定量。结果表明,醋酸氯地孕酮在0.1~50 ng/mL质量浓度范围内线性关系良好,相关系数R2大于0.996,LOD为0.1μg/kg,LOQ为0.3μg/kg。空白样中添加浓度为0.5,2和5μg/kg的醋酸氯孕酮,其平均回收率为68.10%~92.3%,RSD均小于10%。该方法具有操作简便、净化效果显著、灵敏度高、准确性好、检出限低等优点,可用于梅花鹿鹿茸中醋酸氯地孕酮的检测。
An UPLC-MS/MS method was developed for the determination of chlormadinone acetate in pilose antler of sika deer.Antler samples were extracted with acetonitrile and 50 mg PSA purification.Performance liquid chromatography(HPLC)condition was ACQUITY C18 column(2.1 mm×50 mm,1.7μm),mobile phase of acetonitrile,B for water,column temperature 35℃.Mass spectrometry conditions were positive ion mode(ESI+)and multi-reaction monitoring(MRM)mode.The content of chlormadinone acetate in pilose antler was quantitatively determined by external standard method,and the results showed that the linear correlation of chlormadinone acetate was good in the range of 0.1-50 ng/mL,the correlation coefficient R^2 was greater than 0.996,the LOD of chlormadinone acetate was 0.1μg/kg,and LOQ was 0.3μg/kg.The average recovery was 68.10%-92.3%,and RSD was less than 10%with the addition of 0.5,2 and 5μg/kg to chlormadinone acetate in the blank sample.This method had the advantages of simple operation,obvious purification effect,high sensitivity,good accuracy,low detection limit,etc.
作者
黄胜广
赵卉
罗婧
王玉方
刘继永
王峰
HUANG Shengguang;ZHAO Hui;LUO Jing;WANG Yufang;LIU Jiyong;WANG Feng(Institute of Special Animal and Plant Sciences,Chinese Academy of Agricultural Sciences,Changchun 130112)
出处
《食品工业》
CAS
北大核心
2020年第3期285-288,共4页
The Food Industry
基金
特色农产品质量安全风险隐患摸底排查与关键控制点评估(GJFP201701002)。
