气相色谱法同时测定苯酰甲硝唑原料药中乙醇甲苯和吡啶残留量  

Simultaneous Determination of Ethanol,Toluene,and Pyridine Residues in Benzoyl Metronidazole by Gas Chromatography

作　　者：胡忆诺 汪梦蝶 施春阳 张鹰[3] HU Yinuo;WANG Mengdie;SHI Chunyang;ZHANG Ying(Regulatory Affairs,Hubei Hongyuan Pharmaceutical Technology Co.,Ltd, Huanggang 438000,China;Department of Pharmacy,Tongji Hospital,Tongji Medical College, Huazhong University of Science and Technology,Wuhan 430030,China;Department of Pharmacy,Wuhan No.1 Hospital,Wuhan 430022,China)

机构地区：[1]湖北省宏源药业科技股份有限公司注册部,黄冈438000 [2]华中科技大学同济医学院附属同济医院药学部,武汉430030 [3]武汉市第一医院药学部,武汉430022

出　　处：《医药导报》2022年第1期108-111,共4页Herald of Medicine

摘　　要：目的建立苯酰甲硝唑原料药中乙醇、甲苯、吡啶残留量的测定方法。方法采用直接进样法,分析柱为InertCap FFAP毛细管柱(30 m×0.32 mm,0.25μm);程序升温:起始温度为60℃,维持1 min,以4℃·min^(-1)升温至100℃,维持1 min,再以10℃·min^(-1)升温至200℃;采用氢火焰离子化检测器。以外标法计算苯酰甲硝唑中各残留溶剂的量。结果混合对照品溶液和供试品溶液在室温放置8 h稳定性良好;乙醇、甲苯、吡啶的检测限相当于样品浓度分别为7.42,2.54,5.52μg·g^(-1),定量限相当于样品浓度分别为24.74,8.46,18.39μg·g^(-1);当乙醇浓度在50.33~1006.60μg·mL^(-1)范围内,甲苯浓度在8.34~166.88μg·mL^(-1)范围内,吡啶浓度在2.25~45.00μg·mL^(-1)范围内时,乙醇、甲苯、吡啶的浓度与峰面积线性关系良好;乙醇、甲苯、吡啶的回收率分别在92.45%~99.67%,91.92%~99.23%,92.22%~97.61%范围内。结论该方法专属性好、灵敏度高,能有效控制苯酰甲硝唑中乙醇、甲苯、吡啶的残留量。Objective To establish a quality control system of benzoyl metronidazole drug substance,and to establish a gas chromatography(GC)method to determine residual solvents of ethanol,toluene and pyridine in benzoyl metronidazole.Methods The direct injection method was used,and the detection of three residual solvents was performed on a InertCap FFAP capillary column(30 m×0.32 mm,0.25μm)with a temperature program:the initial temperature was 60℃,and it was maintained for 1 minute,raise the temperature to 100℃at 4℃·min^(-1),maintain 1 minute,and then raise the temperature to 200℃at 20℃·min^(-1).The detector was hydrogen flame ionization.The amount of each residual solvent in benzoyl metronidazole was calculated by external standard method.Results The stability of the mixed reference solution and the test solution at room temperature for 8 h was good.The detection limits of ethanol,toluene and pyridine were 7.42,2.54,5.52μg·g^(-1),and the limits of quantification were 24.74,8.46,18.39μg·g^(-1),respectively.When the concentration of ethanol is within the range of 50.33-1006.60μg·mL^(-1),toluene is within the range of 8.34-166.88μg·mL^(-1),and pyridine is within the range of 2.25-45.00μg·mL^(-1),respectively.The concentration of ethanol,toluene,and pyridine has a good linear relationship with the peak area.The recoveries of ethanol,toluene and pyridine were in the range of 92.45%-99.67%,91.92%-99.23%,92.22%-97.61%,respectively.Conclusion This method has good specificity and high sensitivity,and can be used to effectively control the residual amount of ethanol,toluene and pyridine in benzoyl metronidazole.

关 键 词：苯酰甲硝唑 残留溶剂 气相色谱法 

分 类 号：R978[医药卫生—药品] R927.2[医药卫生—药学]