液相色谱串联质谱检测鹿茸及其制品中孕酮等5种性激素

Determination of Five Estrogens in Pilose Antler and Its Products by Liquid Chromatography-tandem Mass Spectrometry

建立了固相萃取-液相色谱-串联质谱法测定鹿茸及其制品中孕酮、睾酮、雌酮、皮质甾酮、17β-雌二醇5种性激素的分析方法。比较了不同提取液对目标物质的提取效果,所测样品经乙腈提取,提取液经HLB固相萃取柱净化,10%甲醇水溶液淋洗杂质,7 mL乙腈洗脱后收集洗脱液氮吹至近干,用1 mL V(甲醇)∶V(0.1%甲酸水溶液)=4∶6复溶,在LC-MS/MS多反应监测(MRM)模式下进行了定性和定量分析。在上述检测条件下,所测的5种性激素的最低检出限均为0.001 mg/kg,平均回收率在87.3%~94.4%之间,RSD在3.87%~7.68%之间,线性范围为0.001~0.2μg/mL,相关系数r>0.999。该方法操作简便,检测结果准确,可以满足鹿茸及其制品中5种性激素的检测要求。

A method for the determination of progesterone,testosterone,estrone,corticosterone and estradiol in human pilose antler and its products by solid phase extraction-liquid chromatography-tandem mass spectrometry was established.Comparing the effect of different reagent extraction,the samples were extracted by acetonitrile and purified by HLB solid phase extraction column.Wash away impurities with the 10% methanol water,collect the eluate after elution with 7 mL acetonitrile,blow it to near dryness,and reconstitute it with 1 mL V(methanol)∶(0.1% formic acid water solution)=4∶6 at the last time.Qualitative and quantitative analysis methods were carried out under the mode of LC-MS/MS multi-reaction monitoring(MRM).Under the above conditions,the minimum detection limit of the five estrogens was 0.001 mg/kg,the average recovery was 87.3%~94.4%,RSD was 3.87%~7.68% and the linear range was 0.001~0.2 μg/mL,r>0.999.The method was simple to operate,the results was accurate and it could be met the requirement detection of 5 kinds of estrogens in pilose antler and its products.