以浙贝母为例研究硫熏炮制新工艺

New Processing Technology of Sulfur Fumigation,Taking Zhebeimu(Fritillariae Thunbergii Bulbus)as an Example

目的:采用高效液相色谱-蒸发光散射检测法(HPLC-ELSD)测定硫磺熏蒸浙贝母的有效成分含量变化,寻找合适的硫熏用硫比例及时间,使其既有利于干燥保存,保证有效成分的含量,又能将二氧化硫残留量控制在合理范围内。方法:色谱柱为Waters XBridge C18色谱柱(250 mm×4.6 mm,5μm);流动相为0.05%二乙胺水溶液(A)-乙腈(B);梯度洗脱(0~5 min,45%B;5~7 min,45%B→25%B;7~18 min,25%B→15%B;18~19 min,15%→45%B;19~22 min,45%B);流速1 mL/min;柱温30℃;漂移管温度60℃;载气流速2.0 L/min。结果:硫熏过后,贝母素甲、贝母素乙、贝母辛含量在一定范围内均增加,但过量硫熏会导致有效成分含量降低。硫熏在一定范围内能增加浙贝母有效成分的含量,且比较适宜的硫熏用量为5.0 g/500 g浙贝母。结论:在合理范围内,硫熏不仅能影响药物的保存,还能影响药物的内在质量,此次对硫熏炮制新工艺的研究,为硫熏工艺标准化提供参考。

Objective:To determine the content changes of the effective components in sulfur fumigation of Zhebeimu(Fritillariae Thunbergii Bulbus) by using HPLC-ELSD,looking for a suitable proportion and time of sulphur fumigation and achieve favorable drying preservation,ensure the content of effective components,control the sulfur dioxide residue within a reasonable range. Methods:Chromatographic column:Waters XBridge C18 column(250 mm×4.6 mm,5 μm);0.01%diethylamine aqueous solution( A)-acetonitrile( B)was used as the mobile phase by gradient elution(0 ~5 min,45% B;5 ~7 min,45%B →25%B;7 ~18 min,25%B→15%B;18 ~19 min,15%→45% B;19~22 min,45%B) at the flow rate of 1 mL·min-1,and the temperatures of column and drift tube were maintained at 30 ℃ and 60 ℃,the carrier gas flow rate was 2.0 L·min-1. Results:After sulfur fumigation,the contents of peimine,peiminine and peimisine increased in a certain range,but excessive sulphur could lead to reduced active ingredient content. Sulfur fumigation could increase the content of effective components in Zhebeimu within a certain range,and the appropriate sulfur fumigation dosage was 5.0 g/500 g of Zhebeimu.Conclusions:In a reasonable range,sulfur fumigation can not only affect the preservation of drugs,but also affect the internal quality of drugs. In this study,the new processing technology of sulfur fumigation was studied to provide reference for the standardization of sulfur fumigation technology.