伤湿止痛膏中硫酸天仙子胺和东莨菪内酯的含量测定研究

Study on the Determination of Hyoscyamine Sulfate and Scopoletin in Shangshi Zhitong Plaster

目的建立HPLC法同时测定伤湿止痛膏中硫酸天仙子胺和东莨菪内酯的含量方法。方法采用WelchΜltimate XB-C18色谱柱(4.6 mm×250 mm,5μm);流动相:0.1%磷酸溶液(A)-乙腈(B)梯度洗脱(0~20 min,13%B;20~35 min,30%B);流速:1.0 mL/min;柱温:25℃;检测波长:210 nm。结果通过对48批不同企业不同批号的伤湿止痛膏产品进行含量测定,拟定每1 cm^(2)伤湿止痛膏中含生物碱以硫酸天仙子胺计,不得少于2.7μg,结果有28批次合格,合格率为58.3%;每1 cm2伤湿止痛膏中含东莨菪内酯不得少于0.18μg,48个批次样品的检测结果均低于限度。结论所建立的方法便捷高效,灵敏度高,可为优化伤湿止痛膏的质量标准提供参考。

Objective To establish a HPLC method for simultaneous determination of hyoscyamine sulfate and scopoletin in shangshi zhitong plaster.Methods Welch Μltimate XB-C18 column(4.6 mm×250 mm,5μm)was used.with the mobile phase consisted of 0.1%phosphoric acid solution(A)-acetonitrile(B)ingradient elution(0-20 min,13%B;20-35 min,30%B);the flow rate was 1.0 mL/min;the temperature of column was 25℃;the detection wavelength was 210 nm.Results According to the content determination of 48 batches of different batches of different enterprises,the alkaloids contained in each 1 cm^(2) of shangshi zhitong plaster were measured by hyoscyamine sulfate,which was not less than 2.7μg.The results showed that 28 batches were qualified,and the pass rate was 58.3%.The content of scopoletin in each 1 cm²shangshi zhitong plaster should not be less than 0.18μg,and the test results of 48 batches of samples were all below the limit.Conclusion The established method is convenient,efficient and sensitive,and can provide reference for optimizing the quality standard of shangshi zhitong plaster.