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高效液相色谱-串联质谱法测定人尿中的3-羟丙基硫醚氨酸

High-performance liquid chromatographic-tandem mass spectrometric determination of 3-hydroxypropylmercapturic acid in human urine.

作者信息

Mascher D G, Mascher H J, Scherer G, Schmid E R

机构信息

Pharm Analyt Laboratory GmbH, Baden, Austria.

出版信息

J Chromatogr B Biomed Sci Appl. 2001 Jan 5;750(1):163-9. doi: 10.1016/s0378-4347(00)00385-6.

Abstract

A sensitive and specific high-performance liquid chromatographic-tandem mass spectrometric (HPLC-MS-MS) method was developed for the determination of 3-hydroxypropylmercapturic acid (3-HPMA) in human urine. Samples were extracted using ENV+ cartridges and then injected onto a C8 Superspher Select B column with acetonitrile and formic acid as eluent (5:95, v/v). N-Acetylcysteine was used as internal standard for HPLC-MS-MS. Linearity was given in the tested range of 50-5000 ng/ml urine. The limit of quantification was 50 ng/ml. Precision, as C.V., in the tested range of 50-5000 ng/ml was 1.47-6.04%. Accuracy ranged from 87 to 114%. 3-HPMA was stable in human urine at 37 degrees C for 24 h. The method was able to quantify 3-HPMA in urine of non-smokers and smokers.

摘要

建立了一种灵敏、特异的高效液相色谱 - 串联质谱法(HPLC-MS-MS)用于测定人尿中的3-羟丙基硫醚氨酸(3-HPMA)。样品采用ENV+柱进行萃取,然后注入以乙腈和甲酸为洗脱剂(5:95,v/v)的C8 Superspher Select B柱。N-乙酰半胱氨酸用作HPLC-MS-MS的内标。在50 - 5000 ng/ml尿液的测试范围内呈线性。定量限为50 ng/ml。在50 - 5000 ng/ml的测试范围内,精密度(以变异系数计)为1.47 - 6.04%。准确度范围为87%至114%。3-HPMA在37℃的人尿中24小时内稳定。该方法能够对非吸烟者和吸烟者尿液中的3-HPMA进行定量。

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