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 C_(18),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10μL。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、8.62～138.0μg/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、1.20μg/mL,检测限分别为0.10、0.19、0.03、0.04、0.42μg/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。
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:HPLCmethod was adopted. The determination was performed on ODS SP C_(18) 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,andcolumn 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 componentswere determined. Relative relational degree(ri)obtained by grey relational analysis method as indexes was used to optimize theprocessing 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 were101.3%,98.7%,99.0%,99.6%,96.4%,respectively(RSD<2.8%,n=6). The results of grey relational analysis showed thatthe relative relational degree(ri)from the processing technology of"boil for 10 min-drying at 50 ℃"was greatest,which hadrelatively small comprehensive effect on the contents of curdione, curcumenol, germacrone, furanodiene and β-elemenerespectively. 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.
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:HPLCmethod was adopted. The determination was performed on ODS SP C_(18) 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,andcolumn 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 componentswere determined. Relative relational degree(ri)obtained by grey relational analysis method as indexes was used to optimize theprocessing 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 were101.3%,98.7%,99.0%,99.6%,96.4%,respectively(RSD<2.8%,n=6). The results of grey relational analysis showed thatthe relative relational degree(ri)from the processing technology of"boil for 10 min-drying at 50 ℃"was greatest,which hadrelatively small comprehensive effect on the contents of curdione, curcumenol, germacrone, furanodiene and β-elemenerespectively. 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.
引文
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[6]唐泽耀,黄靓,林原,等.阿司匹林与β-榄香烯对正常小鼠的凝血时间及缺血心肌模型小鼠的ATP酶活性影响的比较[J].中医药学报,2009,37(5):12-15.
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[12]杨俊杰,张振凌.中药材产地加工与道地药材相关性研究[J].时珍国医国药,2006,17(5):676-677.
[13]周爱珍,程斌,陈玉婷.温郁金加工前后莪术二酮、莪术醇和吉马酮的含量差异研究[J].中华中医药杂志,2016,31(6):129-131.
[14]王胜男,华愉教,邹立思,等.不同加工玄参药材中多元功效成分的含量测定及灰色关联度分析[J].质谱学报,2017,38(3):328-341.
[15]曾颂.基于灰色关联分析法的半夏质效评价研究[D].广州:广东药学院,2013.
[16]张慧,孙秀燕,郑艳萍.RP-HPLC法分离分析温莪术油中6种倍半萜类成分[J].药物分析杂志,2008,28(12):1993-1996.
[17]宋坤,崔小兵,陈建伟,等.GC-MS法分析有氧和充氮加热条件下吉马酮和莪术二酮的化学变化[J].中成药,2014,36(4):808-812.
[18]周阳,陈平,雷敏,等.莪术二酮转化为莪术醇的方法优化[J].武汉轻工大学学报,2017,36(1):30-33.
[2]尹国平,张清哲,安月伟,等.温郁金化学成分及药理活性研究进展[J].中国中药杂志,2012,37(22):3354-3360.
[3]LU JJ,DANG YY,HUANG M,et al.Anti-cancer properties of terpenoids isolated from rhizoma curcumae-a review[J].J Ethnopharmacol,2012,143(2):406-411.
[4]WANG D,HUANG W,SHI Q,et al.Isolation and cytotoxic activity of compounds from the root tuber of curcuma wenyujin[J].Nat Prod Commun,2008,3(6):861-864.
[5]麻杰,陈娟,赵冰洁,等.抗癌药物β-榄香烯及其衍生物的研究进展[J].中草药,2018,49(5):1184-1191.
[6]唐泽耀,黄靓,林原,等.阿司匹林与β-榄香烯对正常小鼠的凝血时间及缺血心肌模型小鼠的ATP酶活性影响的比较[J].中医药学报,2009,37(5):12-15.
[7]唐泽耀,宗成国,林原.莪术醇的活血化瘀活性实验研究[J].中药药理与临床,2003,19(5):15.
[8]王秀.莪术二酮抗血栓和抗血小板聚集作用研究[D].合肥:安徽医科大学,2012.
[9]AN FJ,SUN Y,ZHANG QL,et al.The effects of germacrone on lipopolysaccharide-induced acute lung injury in neonatal rats[J].Cell Mol Biol,2014,60(4):8-12.
[10]谈超,金涌,夏泉.莪术二酮抗炎镇痛作用的实验研究[J].中国骨与关节杂志,2009,8(3):168-170.
[11]CHEN X,ZONG C,GAO Y,et al.Curcumol exhibits anti-inflammatory properties by interfering with the JNK-mediated AP-1 pathway in lipopolysaccharide activated RAW264.7 cells[J].Eur J Pharmacol,2014,723(1):339-345.
[12]杨俊杰,张振凌.中药材产地加工与道地药材相关性研究[J].时珍国医国药,2006,17(5):676-677.
[13]周爱珍,程斌,陈玉婷.温郁金加工前后莪术二酮、莪术醇和吉马酮的含量差异研究[J].中华中医药杂志,2016,31(6):129-131.
[14]王胜男,华愉教,邹立思,等.不同加工玄参药材中多元功效成分的含量测定及灰色关联度分析[J].质谱学报,2017,38(3):328-341.
[15]曾颂.基于灰色关联分析法的半夏质效评价研究[D].广州:广东药学院,2013.
[16]张慧,孙秀燕,郑艳萍.RP-HPLC法分离分析温莪术油中6种倍半萜类成分[J].药物分析杂志,2008,28(12):1993-1996.
[17]宋坤,崔小兵,陈建伟,等.GC-MS法分析有氧和充氮加热条件下吉马酮和莪术二酮的化学变化[J].中成药,2014,36(4):808-812.
[18]周阳,陈平,雷敏,等.莪术二酮转化为莪术醇的方法优化[J].武汉轻工大学学报,2017,36(1):30-33.