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[摘要]
目的 建立葛根中8种主要黄酮类成分UPLC同时测定法,研究超微粉碎技术对葛根黄酮类成分含量的影响,确定葛根超微粉的生产工艺。方法 采用响应面设计方法对葛根粉碎技术中的粉碎时间、投药量和初始粒度3个因素进行考察,以粒径分布(D90、D50)和UPLC法测定的不同粒径葛根粉(10~40、40~65、300目)中8个黄酮类活性成分(3'-羟基葛根素、葛根素、3'-甲氧基葛根素、大豆苷、染料木苷、大豆苷元、染料木素和芒柄花素)的含量数据,共10个指标作为响应因子进行葛根超微粉碎技术评价研究。结果 葛根中8种黄酮类化合物分别在75.8~242.7、205.6~658.0、147.3~417.3、10.2~163.3、11.3~182.0、1.2~18.8、0.25~4.00、0.35~5.37 μg/mL与色谱峰峰面积呈良好的线性关系,平均回收率为98.86%、99.25%、99.90%、100.17%、100.21%、101.40%、100.73%、101.42%,RSD均小于3.0%,UPLC同时测定结果显示,相较其他粒径葛根粉,葛根超微粉(300目)黄酮类含量更高。响应面法优选结果显示超微粉的最佳工艺参数条件为在粒径为80目[(180.0±7.6)μm],通过5号筛时,投药量为247 g,粉碎时间为26 min。结论 响应面法优选的葛根超微粉碎工艺简便,准确度较高,得到的超微粉黄酮含量更高。该工艺可以为葛根超微粉碎技术提供参考。
[Key word]
[Abstract]
Objective To establish simultaneous determination method of eight main flavonoids from Puerariae Lobatae Radix (PLR) by using UPLC, and to study the effect of ultrafine grinding technology on the content of flavonoids in PLR for optimizing its production process. Methods Response surface method was used to investigate the crushing time, sampling capacity, and initial particle size in the superfine pulverizing technology of PLR. Using the particle size distribution (D50, D90), and the content of eight flavonoids (3'-hydroxy puerarin, puerarin, 3'-methoxy puerarin, daidzin, genistin, daidzein, genistein, and formononetin) from PLR powders with various particle sizes (10-40, 40-65, 300 mesh) determined by UPLC, we selected these 10 elements as the response factors to evaluate the ultrafine powders technology for PLR. Results Eight flavonoids from PLR had a good linear relationship with the linear range of 75.8-242.7, 205.6-658.0, 147.3-417.3, 10.2-163.3, 11.3-182.0, 1.2-18.8, 0.25-4.00, 0.35-5.37 μg/mL, and the average recovery ranged from 98.86%, 99.25%, 99.90%, 100.17%, 100.21%, 101.40%, 100.73%, and 101.42%. In addition, the repeatability, stability, and precision RSD were all less than 3%. UPLC result showed that, compared with the PLR powders with other particle sizes, the ultrafine powder of PLR (300 mesh) had a higher flavonoids contents. Results of response surface method showed the optimized preparing parameters of PLR ultrafine powder technology as follows:80 mesh[(180 ±7.6) μm] of particle size, 247 g of sampling amount, and 26 min of crushing time. Conclusion Optimization of ultrafine powders process from PLR by response surface method is simple and accurate, which can obtain PLR ultrafine powder with higher content of flavonoids. This process can provide reference for the ultrafine grinding technology of PLR.
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[基金项目]
国家自然科学基金资助项目(81501229);陕西省科技厅“科技新星”培养计划(2017KJXX-71);陕西省科技统筹创新工程计划项目(2015KTZDSF02-05-02);陕西省创新药物研究中心(2017YWZX-01)