变换波长HPLC法同时测定药食同源降脂片中橙黄决明素、芦丁和槲皮素含量
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摘要
采用Gemini C_(18)色谱柱(4.6 mm×250 mm,5μm),流速为1 mL/min,柱温40℃,波长切换(0～20 min,在370 nm波长下检测芦丁,20～30 min,在280 nm波长下检测槲皮素和橙黄决明素),进样量20μL,流动相为甲醇(A)-水(B)。结果表明,橙黄决明素在1.977 2～98.860 0μg/mL(R~2=0.999 7)线性关系良好,平均回收率为98.81%,RSD为2.0%;芦丁在1.9580～97.9000μg/mL(R~2=0.999 6)线性关系良好,平均回收率为98.16%,RSD为2.2%;槲皮素在2.283 6～114.18μg/mL(R~2=0.999 6)线性关系良好,平均回收率为100.44%,RSD为3.0%。药食同源降脂片中橙黄决明素平均含量0.053 2 mg/g,RSD为1.36%;芦丁平均含量0.847 0 mg/g,RSD为0.65%;槲皮素平均含量0.040 9 mg/g,RSD为0.80%。该方法操作简便、准确、稳定、重复性好,可用于药食同源降脂片的质量控制。
Aurantio-obtusin,rutin and quercetin were separated on Gemini C_(18) RP-column(4.6 mm×250 mm,5 μm),the flow rate was 1.0 mL/min,column temperature was 40 ℃. The detection wavelength was set at 370 nm for rutin 's detection in the first 20 minutes,and then changed into 280 nm for the other two ingredients' s detection in 20～30 minutes. The injection volume was 20 μL,with methyl alcohol as the mobile phase A and water as mobile phase B. Results showed that aurantio-obtusin,rutin and quercetin showed good linear relationships in the range of 1.977 2 to 98.860 0 μg/mL(R~2=0.999 7),1.958 0 to 97.900 0 μg/mL(R~2=0.999 6)and 2.283 6 to 114.18 μg/mL(R~2=0.999 6). Their average recovery rates were 98.81% with RSD of 2.0%,98.16% with RSD of 2.2% and 100.44% with RSD of 3.0%. By measurement,the content of aurantio-obtusin,rutin and quercetin in lipid-lowering Chinese medicines were 0.053 2 mg/g with RSD of 1.36%,0.847 0 mg/g with RSD of 0.65%,and 0.040 9 mg/g with RSD of 0.80%. The method is simple,precise,stable,reproducible,and it can be used for the quality control of lipid-lowering Chinese medicines.
Aurantio-obtusin,rutin and quercetin were separated on Gemini C_(18) RP-column(4.6 mm×250 mm,5 μm),the flow rate was 1.0 mL/min,column temperature was 40 ℃. The detection wavelength was set at 370 nm for rutin 's detection in the first 20 minutes,and then changed into 280 nm for the other two ingredients' s detection in 20～30 minutes. The injection volume was 20 μL,with methyl alcohol as the mobile phase A and water as mobile phase B. Results showed that aurantio-obtusin,rutin and quercetin showed good linear relationships in the range of 1.977 2 to 98.860 0 μg/mL(R~2=0.999 7),1.958 0 to 97.900 0 μg/mL(R~2=0.999 6)and 2.283 6 to 114.18 μg/mL(R~2=0.999 6). Their average recovery rates were 98.81% with RSD of 2.0%,98.16% with RSD of 2.2% and 100.44% with RSD of 3.0%. By measurement,the content of aurantio-obtusin,rutin and quercetin in lipid-lowering Chinese medicines were 0.053 2 mg/g with RSD of 1.36%,0.847 0 mg/g with RSD of 0.65%,and 0.040 9 mg/g with RSD of 0.80%. The method is simple,precise,stable,reproducible,and it can be used for the quality control of lipid-lowering Chinese medicines.
引文
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[13]暴凤伟,刘玉强,张振秋,等.HPLC法测定山楂提取物中芦丁、金丝桃苷、槲皮素的含量[J].中华中医药学刊,2013,31(2):246-248.
[14]张慧月,耿晖,董琼,等.HPLC法同时测定山楂中芦丁和槲皮素含量[J].辽宁中医药大学学报,2016,18(1):64-66.
[15]支国.山楂中主要成分HPLC测定方法的研究[D].河北秦皇岛:河北科技师范学院,2013.
[16]王云霞,张鑫.变换波长HPLC同时测定决明子中橙黄决明素和大黄酚的含量[J].陕西中医,2016(8):1080-1081.
[17]梅国荣,刘飞,王福,等.一测多评法测定决明子中橙黄决明素、大黄素、大黄酚和大黄素甲醚[J].中草药,2016(8):1392-1396.
[18] ZHU L,YU S,ZENG X,et al. Preparative separation and purification of five anthraquinones from Cassia tora L. by highspeed counter-current chromatography[J].Separation and Purification Technology,2008,63(3):665-669.
[2]林嘉成,岑柏宏,江维宁,等.降脂中药活性成分研究进展[J].中国中医药现代远程教育,2013(12):164.
[3]余胜,邓楠,刘文,等.基于代谢组学研究橙黄决明素对高脂血症大鼠的调脂作用[J].分析科学学报,2016,32(2):178-182.
[4]戴迎春.决明子中橙黄决明素的提取分离纯化及在正常大鼠体内的药代动力学参数研究[D].长沙:湖南师范大学,2011.
[5]刘北林,董继生,倪小虎,等.山楂黄酮提取及降血脂研究[J].食品科学,2007,28(5):324-327.
[6]肖婷.山楂对高血脂大鼠模型血脂水平的影响[J].现代医药卫生,2011,27(13):1927-1928.
[7]王玲,吴军林,吴清平,等.山楂降血脂作用和机理研究进展[J].食品科学,2015,36(15):245-248.
[8]林科,张太平,张鹤云.山楂中熊果酸的提取及其对小鼠的降血脂作用[J].天然产物研究与开发,2007,19(6):1052-1054.
[9]易传祝,陈炜林,周月婵.洋葱提取物降血脂动物实验研究[J].中国热带医学,2010,10(5):575-577.
[10]綦振峰,李官浩,郑昌吉,等.山楂、决明子及其配伍的降血脂作用[J].食品与机械,2013(2):96-99.
[11]戴迎春,邓楠,刘文.橙黄决明素在正常大鼠体内的药动学[J].中国医院药学杂志,2015,35(14):1271-1274.
[12]高莹,肖颖.山楂及山楂黄酮提取物调节大鼠血脂的效果研究[J].中国食品卫生杂志,2002,14(3):14-16.
[13]暴凤伟,刘玉强,张振秋,等.HPLC法测定山楂提取物中芦丁、金丝桃苷、槲皮素的含量[J].中华中医药学刊,2013,31(2):246-248.
[14]张慧月,耿晖,董琼,等.HPLC法同时测定山楂中芦丁和槲皮素含量[J].辽宁中医药大学学报,2016,18(1):64-66.
[15]支国.山楂中主要成分HPLC测定方法的研究[D].河北秦皇岛:河北科技师范学院,2013.
[16]王云霞,张鑫.变换波长HPLC同时测定决明子中橙黄决明素和大黄酚的含量[J].陕西中医,2016(8):1080-1081.
[17]梅国荣,刘飞,王福,等.一测多评法测定决明子中橙黄决明素、大黄素、大黄酚和大黄素甲醚[J].中草药,2016(8):1392-1396.
[18] ZHU L,YU S,ZENG X,et al. Preparative separation and purification of five anthraquinones from Cassia tora L. by highspeed counter-current chromatography[J].Separation and Purification Technology,2008,63(3):665-669.