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《化学分析计量》 2022年第07期
DOI:10.3969/j.issn.1008-6145.2022.07.006
气相色谱法同时测定盐酸培唑帕尼中5种有机溶剂
宋小飞,王红芳,宋素丽,柴青叶,陈慧,张辉,游蓉丽
山西振东制药股份有限公司,山西长治 046000 
Simultaneous determination of five organic solvents in pezopanil hydrochloride by gas chromatography
SONG Xiaofei, WANG Hongfang, SONG Suli, CHAI Qingye, CHEN Hui, ZHAN Hui, YOU Rongli
Shanxi Zhendong Pharmaceutical Co., Ltd., Changzhi 046000, China 
摘要:建立同时测定盐酸培唑帕尼原料药中乙醇、异丙醇、乙酸乙酯、碳酸二甲酯、二甲基亚砜5种残留溶剂的方法。用苯甲醇-水(体积比为95∶5)溶液溶解样品,以DB-624毛细管柱(30 m×0.53 mm, 3.0μm)为分离柱,采用氢火焰离子化检测器检测,利用色谱峰面积外标法定量。乙醇、异丙醇、乙酸乙酯、碳酸二甲酯、二甲基亚砜的质量浓度分别在20.01~1 000.59、19.97~998.72、20.11~1 005.71、39.08~195.41、20.14~1 006.98μg/mL范围内与色谱峰面积具有良好的线性关系,相关系数均不小于0.998,检出限为5.99~11.72μg/mL。样品平均加标回收率为90.73%~102.88%,测定结果的相对标准偏差为1.79%~8.31%(n=9)。该方法操作简单,专属性强,耐用性好,可用于测定盐酸培唑帕尼原料药中乙醇、异丙醇、乙酸乙酯、碳酸二甲酯、二甲基亚砜5种残留溶剂。 
Abstract:A method was established to simultaneously determine five residual solvents of ethanol, isopropanol, ethyl acetate, dimethyl carbonate and dimethyl sulfoxide in pezopanib hydrochloride. The sample was dissolved with benzyl alcohol-water (volume ratio was 95∶5) solution, the DB-624 capillary column (30 m×0.53 mm, 3.0μm) was used as the separation column, the hydrogen flame ionization detector was used to detect, and the chromatographic peak area external standard method was used for quantification. The mass concentration of ethanol, isopropanol, ethyl acetate, dimethyl carbonate and dimethyl sulfoxide had a good linear relationship with the chromatographic peak area in the range of 20.01-1 000.59、19.97-998.72、20.11-1 005.71、39.08-195.41、20.14-1 006.98μg/mL respectively, the linear correlation coefficients were not less than 0.998, and the detection limits were 5.99-11.72μg/mL. The recoveries of spiked samples were 90.73%-102.88%, and the relative standard deviations of the determination results were 1.79%-8.31%(n=9). This method is simple to operate, strong in exclusivity and good durability, which can be used to determine five residual solvents of ethanol, isopropanol, ethyl acetate, dimethyl carbonate and dimethyl sulfoxide in pezopani hydrochloride. 
关键词:盐酸培唑帕尼;气相色谱法;残留溶剂;乙醇;异丙醇;乙酸乙酯;碳酸二甲酯;二甲基亚砜 
Keywords:pezopanib hydrochloride; gas chromatography; residual solvent; ethanol; isopropyl alcohol; ethyl acetate;dimethyl carbonate; dimethyl sulfoxide 
本文引用格式:
宋小飞,王红芳,宋素丽,等.气相色谱法同时测定盐酸培唑帕尼中5种有机溶剂[J].化学分析计量,2022,31(7):23.
SONG Xiaofei,WANG Hongfang,SONG Suli,et al. Simultaneous determination of five organic solvents in pezopanil hydrochloride by gas chromatography[J]. Chemical Analysis and Meterage,2022,31(7):23. 

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