温郁金中5种成分的含量测定及其产地加工方法优化
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篇名: 温郁金中5种成分的含量测定及其产地加工方法优化
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摘要: 目的:建立同时测定温郁金中莪术二酮、莪术醇、牻牛儿酮、呋喃二烯、β-榄香烯含量的方法,并优化其产地加工方法。方法:采用高效液相色谱(HPLC)法。色谱柱为ODS SP C18,流动相为乙腈-0.05 %磷酸溶液(梯度洗脱),流速为1.0 mL/min,检测波长为214 nm,柱温为30 ℃,进样量为10 μL。将新鲜温郁金药材经蒸/煮(10、20、30、40 min)、烘干(温度分别为50、60、70 ℃)后制备18批样品药材并测定各批药材中5种成分的含量;以灰色关联分析法得到的相对关联度(ri)为评价指标,优选温郁金药材的最优产地加工方法。结果:莪术二酮、莪术醇、牻牛儿酮、呋喃二烯、β-榄香烯的检测质量浓度线性范围分别为25.56~409.0、2.05~32.8、6.36~102.0、9.14~146.0、8.62~138.0 μg/mL(r均≥0.999 2),精密度、稳定性、重复性试验的RSD均<2.0%(n=6);定量限分别为0.34、0.62、0.11、0.14、1.20 μg/mL,检测限分别为0.10、0.19、0.03、0.04、0.42 μg/mL;平均加样回收率分别为101.3%、98.7%、99.0%、99.6%、96.4%(RSD均<2.8%,n=6);灰色关联分析结果显示,煮10 min-50 ℃烘干的加工方法的ri最大,对温郁金药材中莪术二酮、莪术醇、牻牛儿酮、呋喃二烯、β-榄香烯含量影响最小。结论:HPLC法可用于温郁金药材中5种成分的含量测定,本次优化结果可为温郁金药材产地加工方法的选择提供参考。
ABSTRACT: OBJECTIVE: To establish the method for simultaneous determination of curdione, curcumenol, germacrone, furanodiene and β-elemene in Curcuma wenyujin, and to optimize its processing method in production place. METHODS: HPLC method was adopted. The determination was performed on ODS SP C18 column with mobile phase consisted of acetonitrile-0.05% phosphoric acid solution (gradient elution) at the flow rate of 1.0 mL/min. The detection wavelength was set at 214 nm, and column temperature was 30 ℃. The sample size was 10 μL. 18 batches of sample medicinal materials were prepared by steaming-drying (10, 20, 30, 40 min), or cooking-drying (drying temperature 50, 60, 70 ℃), and then the contents of 5 components were determined. Relative relational degree (ri) obtained by grey relational analysis method as indexes was used to optimize the processing methods of C. wenyujin in production place using. RESULTS: The linear range of curdione, curcumenol, germacrone, furanodiene and β-elemene were 25.56-409.0, 2.05-32.8, 6.36-102.0, 9.14-146.0, 8.62-138.0 μg/mL (r≥0.999 2), respectively. RSDs of precision, stability and reproducibility tests were all lower than 2.0% (n=6). Quantitative limits were 0.34, 0.62, 0.11, 0.14 and 1.20 μg/mL, and detection limits were 0.10, 0.19, 0.03, 0.04 and 0.42 μg/mL, respectively. The average recoveries were 101.3%, 98.7%, 99.0%, 99.6%, 96.4%, respectively (RSD<2.8%, n=6). The results of grey relational analysis showed that the relative relational degree (ri) from the processing technology of “boil for 10 min-drying at 50 ℃” was greatest, which had relatively small comprehensive effect on the contents of curdione, curcumenol, germacrone, furanodiene and β-elemene respectively. CONCLUSIONS: Established HPLC method can be used for content determination of 5 components in C. wenyujin. The results of optimization can provide reference for the selection of processing method of C. wenyujin in production place.
期刊: 2019年第30卷第3期
作者: 周爱珍,鲍珍贝,程斌,朱晓琪
AUTHORS: ZHOU Aizhen,BAO Zhenbei,CHENG Bin,ZHU Xiaoqi
关键字: 温郁金;含量测定;产地加工;高效液相色谱法;灰色关联度分析法
KEYWORDS: Curcuma wenyujin; Content determination; Processing in production place; HPLC; Grey relational analysis method
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