血清和尿液样本中青霉震颤素A和展青霉素C的液相色谱-串联质谱筛查。

LC-MS/MS screen for penitrem A and roquefortine C in serum and urine samples.

作者信息

Tor Elizabeth R, Puschner Birgit, Filigenzi Michael S, Tiwary Asheesh K, Poppenga Robert H

机构信息

California Animal Health and Food Safety Laboratory System, Toxicology Laboratory, University of California, Davis, California 95616, USA.

出版信息

Anal Chem. 2006 Jul 1;78(13):4624-9. doi: 10.1021/ac0601617.

DOI:10.1021/ac0601617

PMID:16808474

Abstract

A rapid LC-MS/MS method, using a triple quadrupole/linear ion trap mass spectrometer, was developed for determination of penitrem A and roquefortine C in serum and urine samples. Penitrem A and roquefortine C were extracted from samples with methylene chloride. The extracts were injected onto a liquid chromatograph coupled with a hybrid triple quadrupole/linear ion trap mass spectrometer. Seven replicate fortifications of serum at 0.001 microg/g (1 ppb) each of penitrem A and roquefortine C gave average recoveries of 90% with 10% CV (relative standard deviation) and 97% with 3% CV, respectively. Seven replicate fortifications of urine at 0.001 microg/g (1 ppb) each of penitrem A and roquefortine C gave average recoveries of 98% with 12% CV and 100% with 6% CV, respectively. This is the first report of a positive mass spectrometric identification and quantitation of both compounds in urine and serum samples from dog intoxication cases.

摘要

建立了一种使用三重四极杆/线性离子阱质谱仪的快速液相色谱-串联质谱法，用于测定血清和尿液样本中的青霉震颤素A和展青霉素C。青霉震颤素A和展青霉素C用二氯甲烷从样本中提取。提取物注入与混合型三重四极杆/线性离子阱质谱仪联用的液相色谱仪。血清中分别以0.001微克/克（1 ppb）的青霉震颤素A和展青霉素C进行七次重复加标，平均回收率分别为90%，变异系数（相对标准偏差）为10%，以及97%，变异系数为3%。尿液中分别以0.001微克/克（1 ppb）的青霉震颤素A和展青霉素C进行七次重复加标，平均回收率分别为98%，变异系数为12%，以及100%，变异系数为6%。这是首次对犬中毒病例的尿液和血清样本中的这两种化合物进行质谱阳性鉴定和定量的报告。