目的 确定大孔吸附树脂纯化延胡索总生物碱的工艺条件。方法 以酸性染料比色法测定延胡索总生物碱，HPLC法测定延胡索中盐酸巴马汀、脱氢紫堇碱、延胡索乙素及延胡索甲素；以延胡索总生物碱和4种生物碱的吸附率、洗脱率及质量分数为指标，利用静态吸附和动态吸附实验相结合的方法，对6种大孔吸附树脂进行筛选。通过考察上样量、体积流量、除杂溶剂和体积、洗脱溶剂和体积等因素，优选延胡索总生物碱纯化工艺条件，以5、10倍放大试验考察纯化工艺的稳定性。结果 选取D141型大孔树脂用于延胡索总生物碱纯化，纯化工艺为生药0.6 g/mL的上样液，加入径高比1∶5～1∶9的D141大孔吸附树脂柱，以体积流量2 BV/h上样2 BV，1.3 BV纯水除杂，6 BV 95%乙醇以2 BV/h体积流量洗脱。纯化后延胡索总生物碱质量分数高达68.19%，盐酸巴马汀、脱氢紫堇碱、延胡索乙素及延胡索甲素的质量分数分别为1.95%、11.74%、4.93%、6.36%。经5、10倍放大试验得到的延胡索总生物碱质量分数能达到65%以上。结论 该工艺经验证试验，总生物碱质量分数能达到65%以上，且延胡索总生物碱及4种生物碱单体的转移率均能达到85%以上，表明D141型大孔吸附树脂能有效纯化延胡索中总生物碱，且适用于工业大生产。

Objective To determine the technological conditions for the purification of the total alkaloid from the Corydalis Rhizoma (CR) by macroporous adsorption resin. Methods Total alkaloids of CR were determined by acid dye colorimetry, palmatine hydrochloride, dehydrocorydaline, tetrahydropalmatine, and corydaline were determined by HPLC. Six macroporous adsorption resins were investigated with the absorption rates, elution rates, and the content of the total alkaloid and four alkaloids of CR by static and dynamic adsorbing experiments. The purification process conditions of the total alkaloid of CR were optimized by the loading amount and volume flow of sample, the type and volume of the impurity removal of solvent and elution solvent and so on. The stability of the purification process was investigated by 5, 10 times enlargement. Results D141 type macroporous adsorption resin was the best choice for the purification of the total alkaloid from CR, the optimized parameters were as follows:Drug concentration was 0.6 g/mL of medicinal material and was added to the D141 macroporous resin column that the ratio of diameter to height range from 1:5 to 1:9 at a flow rate of 2 BV/h to 2 BV, 1.3 BV of purified water was used to remove impurities, and then 6 BV 95% ethanol was used as eluent at a flow rate of 2 BV/h. The purity of the total alkaloid of CR was up to 68.19% after purification, and the content of palmatine hydrochloride, dehydrocorydaline, tetrahydropalmatine, and corydaline was 1.95%, 11.74%, 4.93%, and 6.36%, respectively. The purity of the total alkaloid of the CR can reach more than 65% by 5 times and 10 times enlargement. Conclusion The purity of the total alkaloids can reach more than 65% after verification test, and the transfer rate of total alkaloids and four alkaloid monomers of CR can reach more than 85%, indicating that D141 macroporous adsorption resin can effectively purify total alkaloids from CR, and can be applied to industrial production.

浙江省科学技术厅公益技术研究社会发展项目（2015C33124）；金华市科技局社会发展类重点项目（2015-3-002）