Screening of Nitrosamine Impurities in Sartan Pharmaceuticals by GC-MS/MS

被引：9

作者：

Chang, Shu-Han ^{[1
]}

Ho, Hui-Yu ^{[1
]}

Zang, Chi-Zong ^{[1
]}

Hsu, Ya-Hui ^{[1
]}

Lin, Mei-Chih ^{[1
]}

Tseng, Su-Hsiang ^{[1
]}

Wang, Der-Yuan ^{[1
]}

机构：

[1] Minist Hlth & Welf, Food & Drug Adm, Taipei, Taiwan

来源：

MASS SPECTROMETRY LETTERS | 2021年 / 12卷 / 02期

关键词：

angiotensin II type 1 receptor blockers; carcinogens; gas chromatography; mass spectrometry; nitrosamines; N-NITROSAMINES; DRINKING-WATER; NITROSODIMETHYLAMINE;

D O I：

10.5478/MSL.2021.12.2.31

中图分类号：

O433 [光谱学];

学科分类号：

0703 ; 070302 ;

摘要：

Probable human carcinogenic compounds nitrosamines, have been detected as by-product impurities in sartan pharmaceuticals in recent years which has drawn worries for medication safety. To provide a sensitive and effective method for the quality control of sartan pharmaceuticals, this study established a feasible gas chromatography-tandem mass spectrometry (GC-MS/MS) method for simultaneous determination of 13 nitrosamines. The target analytes were separated on a DB-WAX Ultra Inert column (30 m x 0.25 mm; i.d., 0.25 mu m) and were then subjected to electron impact ionization in multiple reaction monitoring mode. The established method was validated and further employed to analyze authentic samples. Limits of detection (LODs) and limits of quantification (LOQs) of the 13 nitrosamines were 15-250 ng/g and 50-250 ng/g, respectively, which also exhibited intra-day and inter-day accuracies of 91.4-104.8%, thereby satisfying validation criteria. Five nitrosamines, viz., N-nitrosodiethylamine, N-nitrosodimethylamine, N-nitrosodiphenylamine, N-nitrosomorpholine, and N-nitrosopiperidine were detected at concentrations above their LODs in 68 positive samples out of 594 authentic samples from seven sartans.

引用

页码：31 / 40

页数：10

共 30 条

[1]

Alam M.S., 2011, J APPL PHARM SCI, V1, P12

[2] A multi-analyte LC-MS/MS method for screening and quantification of nitrosamines in sartans [J].