泡胆和漂洗炮制环节对黑顺片质量影响研究

Study on the Influence of Bubble Brine Time and Rinsing Times on the quality of Heishunpia

目的研究附子泡胆时间、漂洗次数对黑顺片的质量影响规律,为规范黑顺片炮制提供科学依据。方法采用乙二胺四醋酸二钠滴定法测定附片中的胆巴残留量,应用HPLC法测定附子中双酯型、单酯型生物碱含量,以及参照《中华人民共和国药典》(2015年版)四部2201热浸法测定附片中水溶性浸出物。结果泥附子泡胆20天后钙离子含量趋于平衡,平均含量为9.21%~9.39%;泡胆10~106天水溶性浸出物无明显趋势变化,平均含量为67%~73%,双酯型生物碱由0.058%下降至0.029%,单酯型生物碱基本稳定不变平均含量为0.014%~0.018%。附片漂洗1~5次,胆巴残留量由平均3.86%下降至0.73%,单酯型生物碱由0.027%下降至0.011%,水溶性浸出物由29%下降至12%,双酯型生物碱漂洗1次后含量至0.013%以下。结论泡胆能有效降低毒性双酯型生物碱含量,随着漂洗次数的增加,浸出物、生物碱含量、胆巴残留量逐渐降低。为有效保证黑顺片饮片的安全有效,建议泥附子泡胆应控制在20天以上,漂洗3~4次为宜。

Objective The effects of bubble brine time and rinsing times of Fuzi on the quality of Heishunpian were studied, which provided scientific basis for standardizing the processing of Heishunpian. Methods The residual bile bar in Fuzi was determined by disodium ethylenediamine tetraacetate titration, the contents of diester and monoester alkaloids in aconite were determined by HPLC, and the water soluble leachate was determined by hot leaching with reference to the Pharmacopoeia of the peopleu Republic of China(2015 edition).Results Soak gall bladder in aconite for 20 days later, the calcium ion content of the aconite was balanced, the average content was 9.21% ~ 9.39%. The water-soluble extract of the foam from 10 to 106 days showed no obvious difference, the average content was 67 %~ 73%, the content of diester type alkaloids decreased from 0.058% to 0.029%, and the basic stability of monoester-type alkaloids was 0.014 %~ 0.018%. After 1 ~ 5 times of rinsing, the residual amount of the bile pigment decreased from 3.86% to 0.73%, the monoester type alkaloid decreased from 0.027% to 0.011%, the water-soluble extract decreased from 29% to 12%, and the content of the double ester type alkaloid was less than 0.013%.Conclusion Bubble bile can effectively reduce the content of toxic diester alkaloids. With the increase of rinsing times, the leachate, alkaloid content and cholbar residue decrease gradually. In order to effectively ensure the safety and effectiveness of Heishunpian, it is suggested that the bubble gall of aconite should be controlled for more than 20 days and rinsed 3 times to 4 times.