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YIN Lining, ZHANG Yu, HU Yiqiao, ZHAN Xin'an. GC-MS method for the determination of the genotoxic impurity chlorocyclohexane in trihexyphenidyl hydrochloride bulk drug[J]. Journal of China Pharmaceutical University, 2022, 53(1): 79-85. DOI: 10.11665/j.issn.1000-5048.20220112
Citation: YIN Lining, ZHANG Yu, HU Yiqiao, ZHAN Xin'an. GC-MS method for the determination of the genotoxic impurity chlorocyclohexane in trihexyphenidyl hydrochloride bulk drug[J]. Journal of China Pharmaceutical University, 2022, 53(1): 79-85. DOI: 10.11665/j.issn.1000-5048.20220112
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GC-MS method for the determination of the genotoxic impurity chlorocyclohexane in trihexyphenidyl hydrochloride bulk drug

  • 1.

    School of Life Sciences, Nanjing University, Nanjing 210093

  • 2.

    Hisun Pharmaceutical (Hangzhou) Co., Ltd., Hangzhou 311404, China

Funds: This study was supported by the National Natural Science Foundation of China (No.31872755,No.81872811), Jiangsu Outstanding Youth Fund (No.BK20190007) and the Central Fundamental Research Funds for the Central Universities (No.02141438473)
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  • Received Date: May 26, 2021
  • Revised Date: January 05, 2022
    Graphical Abstract
    • 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.
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    • References (9)
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