GC-MS method for the determination of the genotoxic impurity chlorocyclohexane in trihexyphenidyl hydrochloride bulk drug
10.11665/j.issn.1000-5048.20220112
- VernacularTitle:GC-MS法测定盐酸苯海索原料药中遗传毒性杂质氯代环己烷
- Author:
Lining YIN
1
;
Yu ZHANG
;
Yiqiao HU
;
Xin'an ZHAN
Author Information
1. 南京大学生命科学学院
- Publication Type:Journal Article
- Keywords:
trihexyphenidyl hydrochloride;
chlorocyclohexane;
genotoxic impurity;
GC-MS;
trace analysis
- From:
Journal of China Pharmaceutical University
2022;53(1):79-85
- CountryChina
- Language:Chinese
-
Abstract:
Gas chromatography-mass spectrometry (GC-MS) method was established for trace analysis of the potential genotoxic impurity chlorocyclohexane in trihexyphenidyl hydrochloride bulk drug, utilizing an RXI-5SIL MS column at isothermal temperature of 60 °C for the entire 6-minute run time.The inlet temperature was 180 °C and a split ratio of 10∶1 was used with the injection volume of 1.0 μL.The selective ion monitoring mode was set at m/z 82 for chlorocyclohexane with a detector voltage of 0.3 kV and an ion source temperature of 240 °C.The method was verified with respect to specificity, limit of detection (LOD), limit of quantitation (LOQ), accuracy, precision and robustness.Good linear correlation was achieved with coefficient r of 0.999 9 in the concentration range of 59.72-493 ng/mL.The intra- and inter-day precision was satisfactory (RSD ≤ 5.0%) and robust (RSD ≤ 1.65%).The proposed method in this study can be adequately adopted as a tool for quality assurance of trihexyphenidyl hydrochloride in routine test of potential genotoxic impurity.
