HPLC法测定抗痨散中芥子碱硫氰酸盐的含量

摘要

Objective To establish the method to determine the content of sinapine thiocyanate in the hospital preparation of anti-tuberculosis pulvis.Methods According to the high performance liquid chromatography (HPLC) described in Volume Ⅳ of Chinese Pharmacopoeia (2015),the acetonitrile-0.08 mol/L potassium dihydrogen phosphate solution (12∶88) was taken as the mobile phase;the Shimadzu inertsustain C18 column (250 mmx4.6 mm,5 μm) was used;the detection wavelength was 326 nm and the injection volume was 20 μl.Under such chromatographic condition,the content of sinapine thiocyanate in the anti-tuberculosis pulvis was measured and tests were performed for the precision,repeatability,stability and recovery rate.Results Within the range of 0.00509-0.08129 mg/ml,there was a good linear relationship between the content of sinapine thiocyanate and the peak area.The relative standard deviation(RSD) of precision and repeatability was 0.57％ and 1.53％ respectively;the average recovery rate of sample was 95.58％ and the RSD was 1.70％.Conclusion The HPLC method can accurately monitor the content of sinapine thiocyanate in anti-tuberculosis pulvis.%目的 建立医院制剂抗痨散中芥子碱硫氰酸盐含量测定的方法.方法 依据《中国药典》2015年版一部通则高效液相色谱法(HPLC),以乙腈-0.08 mol/L磷酸二氢钾溶液(12∶88)为流动相;色谱柱:岛津inertsustain C18(250 mm×4.6 mm,5 μm);检测波长326 nm;进样量20μl.在此色谱条件下,检测抗痨散中芥子碱硫氰酸盐含量,并进行精密度、重复性、稳定性、回收率试验.结果 在0.00509～0.08129 mg/ml范围内,芥子碱硫氰酸盐含量与峰面积呈良好的线性关系,精密度、重复性RSD分别为0.57％、1.53％;样品平均回收率为95.58％,RSD为1.70％.结论 HPLC法能准确监测抗痨散中芥子碱硫氰酸盐的含量.