摘要
目的:建立同时测定藏药四味姜黄汤中10种有效成分的含量,并对其煎煮工艺进行优化。方法:采用高效液相色谱法测定含量。以浸泡时间、加水量、煎煮时间、煎煮次数为考察因素,10种成分的含量及出膏率的综合得分为响应值,在单因素试验的基础上,采用Box-Behnken响应面法优化其煎煮工艺。结果:没食子酸、柯里拉京、木兰花碱、鞣花酸、盐酸药根碱、盐酸巴马汀、盐酸小檗碱、双去甲氧基姜黄素、去甲氧基姜黄素、姜黄素进样量的线性范围分别为0.280 6~1.683 6、0.289 6~1.737 6、0.320 8~1.924 8、0.116 0~0.696 0、0.018 9~0.113 5、0.013 3~0.079 9、0.092 3~0.553 8、0.025 5~0.153 0、0.036 1~0.216 3、0.041 0~0.245 7μg(r均为0.999 9);定量限分别为0.28、14.48、3.21、11.60、1.89、4.44、0.46、0.26、0.36、0.41 ng,检测限分别为0.11、4.14、1.24、3.32、0.58、1.33、0.13、0.09、0.14、0.12 ng;精密度、稳定性、重复性试验的RSD均小于3%;加样回收率为92.56%~103.69%(RSD为0.90%~3.81%,n=6)。该方的最优煎煮工艺为浸泡60 min,加入8倍量(mL/g)水,煎煮2次,每次65 min。6次验证试验中,综合得分为3.323 2~3.422 4分,与预测值(3.437 4)相对误差的绝对值均小于2%。结论:所建含量测定方法操作简单,重复性较好,可用于同时测定四味姜黄汤中10种有效成分的含量;优化所得煎煮工艺稳定、可行。
OBJECTIVE:To establish the method for simultaneous determination of 10 kinds of active components in Tibetan medicine Siwei jianghuang prescription,and to optimize its decoction technology. METHODS:HPLC method was adopted. Using soaking time,the amount of added water,decoction time and decoction times as factors,comprehensive score of the contents of10 kinds of components and solid extracts rate as response values,one the basis of single factor test,Box-Behnken response surface method was used to optimize its decoction technology. RESULTS:The linear range of gallic acid,corilagin,magnoflorine,ellagic acid, hydrochloric jatrorrhizine, hydrochloride palmatine, hydrochloride berberine, bisdemethoxycurcumin,demethoxycurcumin and curcumin were 0.280 6-1.683 6,0.289 6-1.737 6,0.320 8-1.924 8,0.116 0-0.696 0,0.018 9-0.113 5,0.013 3-0.079 9,0.092 3-0.553 8,0.025 5-0.153 0,0.036 1-0.216 3,0.041 0-0.245 7 μg(all r were 0.999 9),respectively. The limits of quantitation were 0.28,14.48,3.21,11.60,1.89,4.44,0.46,0.26,0.36,0.41 ng,respectively. The limits of detection were 0.11,4.14,1.24,3.32,0.58,1.33,0.13,0.09,0.14,0.12 ng,respectively. RSDs of precision,stability and reproducibility tests were all lower than 3%. The recoveries were 92.56%-103.69%(RSDs were 0.90%-3.81%,n=6). The optimal decoction technology included soaking 60 min,adding 8-fold(mL/g) water,decoction for twice,lasting for 65 min each time. In 6 validation tests,comprehensive scores were 3.323 2-3.422 4,and the absolute value of the relative error with the predicted value(3.437 4)was less than 2%.CONCLUSIONS:Established method is simple and repeatable,and can be used for simultaneous determination of 10 kinds of active components in Siwei jianghuang prescription. Optimized decoction technology is stable and feasible.
作者
王小艳
向宇楠
高洁
潘琳
毕若红
赖先荣
李啟恩
李先加
WANG Xiaoyan;XIANG Yunan;GAO Jie;PAN Lin;BI Ruohong;LAI Xianrong;LI Qi’en;LI Xianjia(College of Pharmacy,Chengdu University of TCM,Chengdu 611137,China;Tibetan Medical College,Qinghai University,Xining 810016,China)
出处
《中国药房》
CAS
北大核心
2020年第8期913-919,共7页
China Pharmacy
基金
国家自然科学基金资助项目(No.81774007,No.815-60806,No.81473427,No.81173360)
国家重点研发计划中医药现代化研究重点专项(No.2017YFC1703900)
青海省科技计划项目(No.2017-ZJ-922Q)
四川省教育厅重点项目(No.16ZA0120)。
