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LC–MS/MS procedure for the simultaneous determination of N-acetyl-S-(1-naphthyl)cysteine and N-acetyl-S-(2-napthyl)cysteine in human urine
Journal of Chromatography B ( IF 3 ) Pub Date : 2017-12-16 , DOI: 10.1016/j.jchromb.2017.12.023
Melanie Zobel , Katrin Klotz , Thomas Göen

A two-dimensional liquid chromatographic electrospray-ionization tandem mass spectrometric (LC/LC–ESI–MS/MS) procedure for the simultaneous determination of the expected mercapturic acids of naphthalene (1- and 2-naphthylmercapturic acids; 1- and 2-NpMA) and of the well-established parameter for benzene biomonitoring (S-phenylmercapturic acid; PhMA) in human urine was developed, validated and applied to human urine samples. Apart from sample acidification, the enrichment of analytes and sample clean-up as well as the separation of all analytes were completely automated using both a restricted access material column (RAM C18) and a core-shell biphenyl material. Sensitive, specific and reliable detection of all target substances, with limits of detection ranging from 0.03 to 0.04 μg/L, was achieved using structurally well matching isotope-labelled internal standard substances for each analyte. Intraday and interday precision were determined, ranging from 2.2 to 4.3%, and mean accuracy from 98.4 to 100.8%. Due to the low limits of detection, the good precision and accuracy of the developed procedure, it is well suited for application in biomonitoring studies to evaluate the validity of mercapturic acids as biomarkers after naphthalene exposure.



中文翻译:

LC-MS / MS方法同时测定人尿中的N-乙酰基-S-(1-萘基)半胱氨酸和N-乙酰基-S-(2-萘基)半胱氨酸

二维液相色谱电喷雾电离串联质谱(LC / LC–ESI–MS / MS)方法,用于同时测定萘的预期巯基酸(1-和2-萘巯基酸; 1-和2-NpMA )和已建立的苯生物监测参数(S-苯硫醇酸;开发,验证并应用于人尿液中的PhMA)。除了样品酸化以外,使用受限通道进样柱(RAM C18)和核-壳联苯材料均可完全自动化分析物的富集和样品净化以及所有分析物的分离。使用结构良好匹配的同位素标记的内标物对每种分析物实现了对所有目标物质的灵敏,特异和可靠的检测,检测范围为0.03至0.04μg/ L。确定了日内和日间精度,范围为2.2到4.3%,平均精度为98.4到100.8%。由于检测限低,开发的程序具有良好的精度和准确性,

更新日期:2017-12-16
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