HPLC-ELSD法测定青霉胺片的含量

Determination of penicillamine tablets by HPLC-ELSD

目的:建立青霉胺片含量测定的HPLC-ELSD法。方法:采用Apollo C_(18)色谱柱(4.6 mm×250 mm,5μm),流动相为0.1 mol·L^(-1)三氟乙酸溶液-乙腈(91∶9),柱温25℃,进样量20μL。ELSD低温分流模式检测:漂移管温度65℃,载气流速1.5 L·min^(-1),增益2。结果:青霉胺在0.964~2.972 mg·mL^(-1)浓度范围内,浓度对数与峰面积对数线性关系良好;加标回收率结果为99.4%~102.1%,平均回收率100.0%;各辅料与青霉胺均能有效分离;定量限为0.159μg。31批次青霉胺片测定结果为97.1%~101.5%,服从正态分布。结论:本法操作简单,专属性强,准确度及精密度良好,对环境污染较小。

Objective:To establish an HPLC-ELSD method for the determination of penicillamine tablets.Methods:The column was Apollo C_(18)(4.6 mm×250 mm,5μm)maintained at 25℃.The mobile phase was 0.1 mol·L^(-1) trifluoroacetic acid solution:methanol(91∶9),and the injection was 20μL.ELSD conditions were as follows,drift tube temperature of 65℃,carrier gas flow rate of 1.5 L·min^(-1),and gain of 2.Results:In the concentration range of 0.964-2.972 mg·mL^(-1),logarithm of concentration and logarithm of peak area had a good linear relationship,and the recovery was 99.4%-102.1% with an average recovery of 100.0%.The excipients and penicillamine were separated effectively and the quantitative limit was 0.159μg.The content results of 31 batches of penicillamine tablets were from 97.1% to 101.5%,which followed normal distribution.Conclusion:The method is simple in operation,strong in specificity,good in accuracy and precision,and less in environmental pollution.