Determination of α-amanitin in serum and liver by multistage linear ion trap mass spectrometry
Determination of α-amanitin in serum and liver by multistage linear ion trap mass spectrometry
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DOI：
10.1021/jf063194w
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发表时间：
2007-04-18
影响因子：
6.1
通讯作者：
Puschner, Birgit
中科院分区：
文献类型：
--
作者：
Filigenzi, Michael S.;Poppenga, Robert H.;Puschner, Birgit
本文采用LC-MS/MS/MS法快速分析血清和肝脏中的α-氨基甲酸甘油酯。血清最初是用乙腈沉淀蛋白质，然后用二氯甲烷除去乙腈。用乙腈水溶液匀浆制备肝脏，然后用二氯甲烷去除乙腈。对于这两种基质，水相用混合模式C18/阳离子交换固相萃取柱提取，并在线性离子陷阱LC-MS系统上进行分析。以对照矩阵提取液制备标准品。以0.001 mg/g(1 ng/g)添加7次血清，平均回收率为95%，相对标准偏差为8.8%(RSD)，计算方法检出限为0.26 ng/g，以1 ng/g添加7次对照肝脏，平均回收率为98%，变异系数为17%，计算方法检出限为0.5 ng/g。
This paper describes a rapid LC-MS/MS/MS method for the analysis of alpha-amanitin in serum and liver. Serum was initially prepared by precipitation of proteins with acetonitrile and subsequent removal of acetonitrile with methylene chloride. Liver was prepared by homogenization with aqueous acetonitrile and subsequent removal of acetonitrile using methylene chloride. For both matrices, the aqueous phase was then extracted using mixed-mode C18/cation exchange SPE cartridges and analyzed on a linear ion trap LC-MS system. Standards were prepared in extracts of control matrix. Seven replicate fortifications of serum at 0.001 mu g/g (1 ng/g) of alpha-amanitin gave a mean recovery of 95% with 8.8% CV (relative standard deviation) and a calculated method detection limit of 0.26 ng/g. Seven replicates of control liver fortified at 1 ng/g gave a mean recovery of 98% with 17% CV and a calculated method detection limit of 0.50 ng/g. This is the first report of a positive mass spectrometric identification and quantitation of alpha-amanitin in serum and liver from suspect human and animal intoxications.