加校正因子的主成分自身对照法同时测定利培酮中2种氧化性杂质

目的:建立加校正因子的主成分自身对照法测定利培酮中2种氧化性杂质的含量。方法:采用ZORB-AX Extend C₁₈(4.6 mm×250 mm,5μm)色谱柱,以流动相A:0.1%三氟乙酸溶液-乙腈(80∶20)(用氨水调pH 3.0)和流动相B:0.1%三氟乙酸溶液-甲醇(61∶39)(用氨水调pH 3.0)作为流动相,梯度洗脱,流速为2.5 mL·min^-1,检测波长为275 nm,进样量为10μL,柱温为30℃。测定利培酮与2种氧化性杂质的标准曲线方程,以斜率比值计算氧化性杂质相对于利培酮的校正因子,用系统适用性试验溶液结合相对保留时间对氧化性杂质进行定位。结果:2种氧化性杂质的相对保留时间分别为1.55与1.71,校正因子分别为1.14与1.15。结论:本方法可用于利培酮中2种氧化性杂质的定性及定量分析,采用加校正因子的主成分自身对照法更加准确测定2种氧化性杂质的含量。

The principal component self-compare with correction factor method for determination of related substances in risperidone

Objective:To establish the principal component self-compare with correction factor method to determine the contents of oxidizing impurities in risperidone.Methods:Analysis was carried out on a ZORBAX Extend C₁₈column(4.6 mm×250 mm,5μm).The mobile phase A was 0.1%trifluoroacetic acid solution-acetonitrile(80∶20)(pH adjusted to 3.0 with ammonia solution),and the mobile phase B was 0.1%trifluoroacetic acid solution-methanol(61∶39)(pH adjusted to 3.0 with ammonia solution).The detection wave length was 275 nm,the column temperature was 30℃,and the injection volume was 10μL.The slope of linear equation was used to determine the relative correction factor between oxidizing impurities and risperidone.The system suitability test solution combined with relative retention time was used to locate the oxidizing impurities.Results:The relative retention time values of oxidizing impurities were 1.55 and 1.71,respectively.The relative correction factor values o oxidizing impurities were 1.14 and 1.15,respectively.Conclusion:The method can be used for the qualitative and quantitative analysis of oxidizing impurities in risperidone,and the principal component self-control method with correction factor is more accurate for the determination of two oxidizing impurities.