正交试验优选细叶铁线莲醇提工艺  

Optimization of Ethanol Extraction Process of Herba Clematis by Orthogonal Test

作　　者：王回霞 谢和兵 尼玛次仁 白玛旦增 WANG Huixia;XIE Hebing;NIMA Ciren;BAIMA Danzeng(School of Pharmacy,Anhui University of Chinese Medicine,Hefei,Anhui,China 230012;Yangtze Delta Drug Advanced Research Institute,Nantong,Jiangsu,China 226133;Jiangsu God Monkey Medical Research Co.,Ltd.,Nantong,Jiangsu,China 226133;Tibet God Monkey Pharmaceutical Co.,Ltd.,Shigatse,Xizang,China 857000)

机构地区：[1]安徽中医药大学药学院,安徽合肥230012 [2]江苏省南通市海门长三角药物高等研究院,江苏南通226133 [3]江苏神猴医药研究有限公司,江苏南通226133 [4]西藏神猴药业有限责任公司,西藏日喀则857000

出　　处：《中国药业》2024年第14期66-70,共5页China Pharmaceuticals

基　　金：西藏自治区日喀则市区域科技协同创新专项[QYXTZX-RKZ2022-07]。

摘　　要：目的 优选细叶铁线莲的醇提工艺。方法 采用高效液相色谱法测定细叶铁线莲饮片样品中槲皮素的含量;以紫外吸收光谱法测定饮片样品中总黄酮含量;以料液比、提取次数、提取时间为考察因素,以干膏得率、总黄酮含量和槲皮素含量为考察指标,采用L9(3~4)正交试验法优选最佳醇提工艺,并验证。结果 槲皮素质量浓度在1.99~198.99μg/mL范围内与峰面积线性关系良好(r=0.999 9,n=6),定量限和检测限分别为0.060μg/mL和0.018μg/mL;精密度、稳定性和重复性试验结果的RSD均小于2.0%;平均加样回收率为101.74%,RSD为1.25%(n=6)。芦丁质量浓度在7.42~44.52μg/mL范围内与吸光度线性关系良好。最佳工艺条件为加10倍40%乙醇,提取3次,每次0.5 h。验证试验中干膏得率、总黄酮含量、槲皮素含量分别为25.10%,56.78 mg/g,1.35 mg/g,RSD分别为2.43%,4.10%,2.13%(n=3)。结论 该研究中优选的醇提工艺稳定可靠、重复性好,可为细叶铁线莲的质量评价及其制剂产品的产业化开发提供参考。Objective To optimize the ethanol extraction process of Herba Clematis.Methods The high-performance liquid chromatography(HPLC)method was used to determine the content of quercetin in the Herba Clematis Decoction Piece samples,and the ultraviolet absorption spectroscopy was used to determine the content of total flavonoids in the decoction piece samples.The ethanol extraction process of Herba Clematis was optimized by the L9(34)orthogonal test with the ratio of material to liquid,extraction frequency and extraction time as the investigation factors,and with the yield of dry extract,total flavonoid content and quercetin content as the investigation indicators.Then the verification test was conducted.Results The mass concentration of quercetin showed a good linear relationship with the peak area in the range of 1.99-198.99μg/mL(r=0.9999,n=6).The limit of quantification and the limit of detection were 0.060μg/mL and 0.018μg/mL respectively.The RSDs of precision,stability and repeatability tests were all lower than 2.0%.The average recovery rate of quercetin was 101.74%with an RSD of 1.25%(n=6).The mass concentration of rutin showed a good linear relationship with the absorbance in the range of 7.42-44.52μg/mL.The optimal process was as follows:adding 10 times of 40%ethanol,extracting three times,each time for 0.5 h.The yield of dry extract,total flavonoid content and quercetin content in the the verification test were 25.10%,56.78 mg/g,1.35 mg/g,with the RSDs of 2.43%,4.10%,2.13%(n=3),respectively.Conclusion The optimal ethanol extraction process in this study is stable,reliable and repeatable,which can provide a reference for the quality evaluation of Herba Clematis and the industrial development of its preparation products.

关 键 词：细叶铁线莲 醇提工艺 槲皮素 高效液相色谱法 正交试验法 含量测定 

分 类 号：R943[医药卫生—药剂学]