HPLC法同时测定沉香化滞丸中11种成分
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摘要
目的采用HPLC梯度洗脱法同时测定沉香化滞丸中沉香四醇、柚皮苷、橙皮苷、新橙皮苷、和厚朴酚、大黄素、厚朴酚、木香烃内酯、去氢木香内酯、大黄酚、大黄素甲醚11种成分。方法采用Thermo Syncronis C18色谱柱(250 mm×4.6 mm,5μm),流动相为水-乙腈,梯度洗脱:0～10 min,20%乙腈;10～20 min,20%～40%乙腈;20～24 min,40%乙腈;24～26 min,40%～52%乙腈;26～30 min,52%乙腈;30～31 min,52%～90%乙腈;31～35 min,90%乙腈;35～40 min,90%～100%乙腈;40～43min,100%乙腈;43～45min,100%～20%乙腈;检测波长215nm,体积流量1.0m L/min,柱温30℃,进样量20μL。结果各成分在43 min内分离良好,沉香四醇、柚皮苷、橙皮苷、新橙皮苷、和厚朴酚、大黄素、厚朴酚、木香烃内酯、去氢木香内酯、大黄酚、大黄素甲醚的线性范围分别为1.4～13.6、10.0～200.0、31.5～315.0、1.0～120.1、1.8～50.6、0.93～10.1、1.8～30.0、0.2～40.3、1.8～18.1、1.7～25.0、0.45～10.70μg/mL;样品中各成分的平均回收率均在98.90%～100.87%;11种成分精密度RSD在0.55%～1.54%;供试品溶液在30 h内稳定性良好,RSD在0.75%～1.94%;重复性RSD在0.39%～1.73%。6批次样品中沉香四醇、柚皮苷、橙皮苷、新橙皮苷、和厚朴酚、大黄素、厚朴酚、木香烃内酯、去氢木香内酯、大黄酚、大黄素甲醚质量分数分别为92.0～201.0、511.5～9 033.0、5 475.0～12 635.5、54.5～5 095.5、192.0～2 137.5、117.0～391.5、106.5～1 281.5、13.0～136.5、93.5～199.0、177.0～1 207.0、33.5～251.5μg/g。结论本方法准确、快速、简便,重复性好,精密度高,适用于沉香化滞丸中多种活性成分的定量分析。
Objective To develop an HPLC method for simultaneous determination of the eleven constituents(agaric-alcohol,naringin, hesperidin, neohesperidin, honokiol, emodin, magnolol, costunolide, dehydrocostus, chrysophanol, and physcion) in Chenxiang Huazhi Pills(CHP) by HPLC with gradient elution. Methods The chromatographic separation was performed on an Thermo Syncronis C18 column(4.6 mm × 250 mm, 5 μm) which was operated at 30 ℃. The mobile phase was a linear gradient prepared from water(A) and acetonitrile(B). The linear gradient elution program was programmed as follows: 0—10 min, 20%acetonitrile; 10—20 min, 20%—40% acetonitrile; 20—24 min, 40% acetonitrile; 24—26 min, 40%—52% acetonitrile; 26—30 min,52% acetonitrile; 30—31 min, 52%—90% acetonitrile; 31—35 min, 90% acetonitrile; 35—40 min, 90%—100% acetonitrile; 40—43 min, 100% acetonitrile; 43—45 min, 100%—20% acetonitrile. The flow rate was 1 mL/min and the detection wavelength was 215 nm.Results The analysis permitted very good separation of eleven constituents within 43 min. A good linear relationship between the peak area and the injection volume was obtained. The ranges of the eleven constituents were 1.4—13.6, 10.0—200.0, 31.5—315.0,1.0—120.1, 1.8—50.6, 0.93—10.1, 1.8—30.0, 0.2—40.3, 1.8—18.1, 1.7—25.0, and 0.45—10.70 μg/mL. The average recoveries of eleven constituents in the samples were in the range of 98.90%—100.87%. The precision RSD of the peak areas of the 11 components ranged from 0.55%—1.54%; Eleven components had good stability within 30 h, and the concentration RSD of each component ranged from 0.75% to 1.94%; The repeatability RSD of each component ranged from 0.39% to 1.73%. The content of agaric-alcohol, naringin,hesperidin, neohesperidin, honokiol, emodin, magnolol, costunolide, dehydrocostus, chrysophanol, and physcion in six batches were92.0—201.0, 511.5—9 033.0, 5 475.0—12 635.5, 54.5—5 095.5, 192.0—2 137.5, 117.0—391.5, 106.5—1 281.5, 13.0—136.5,93.5—199.0, 177.0—1 207.0, and 33.5—251.5 μg/g, respectively. Conclusion The method is accurate, rapid and simple with high sensitivity, precision and repeatability, which has been successfully applied as an effective tool for the multicomponent analysis of CHP.
Objective To develop an HPLC method for simultaneous determination of the eleven constituents(agaric-alcohol,naringin, hesperidin, neohesperidin, honokiol, emodin, magnolol, costunolide, dehydrocostus, chrysophanol, and physcion) in Chenxiang Huazhi Pills(CHP) by HPLC with gradient elution. Methods The chromatographic separation was performed on an Thermo Syncronis C18 column(4.6 mm × 250 mm, 5 μm) which was operated at 30 ℃. The mobile phase was a linear gradient prepared from water(A) and acetonitrile(B). The linear gradient elution program was programmed as follows: 0—10 min, 20%acetonitrile; 10—20 min, 20%—40% acetonitrile; 20—24 min, 40% acetonitrile; 24—26 min, 40%—52% acetonitrile; 26—30 min,52% acetonitrile; 30—31 min, 52%—90% acetonitrile; 31—35 min, 90% acetonitrile; 35—40 min, 90%—100% acetonitrile; 40—43 min, 100% acetonitrile; 43—45 min, 100%—20% acetonitrile. The flow rate was 1 mL/min and the detection wavelength was 215 nm.Results The analysis permitted very good separation of eleven constituents within 43 min. A good linear relationship between the peak area and the injection volume was obtained. The ranges of the eleven constituents were 1.4—13.6, 10.0—200.0, 31.5—315.0,1.0—120.1, 1.8—50.6, 0.93—10.1, 1.8—30.0, 0.2—40.3, 1.8—18.1, 1.7—25.0, and 0.45—10.70 μg/mL. The average recoveries of eleven constituents in the samples were in the range of 98.90%—100.87%. The precision RSD of the peak areas of the 11 components ranged from 0.55%—1.54%; Eleven components had good stability within 30 h, and the concentration RSD of each component ranged from 0.75% to 1.94%; The repeatability RSD of each component ranged from 0.39% to 1.73%. The content of agaric-alcohol, naringin,hesperidin, neohesperidin, honokiol, emodin, magnolol, costunolide, dehydrocostus, chrysophanol, and physcion in six batches were92.0—201.0, 511.5—9 033.0, 5 475.0—12 635.5, 54.5—5 095.5, 192.0—2 137.5, 117.0—391.5, 106.5—1 281.5, 13.0—136.5,93.5—199.0, 177.0—1 207.0, and 33.5—251.5 μg/g, respectively. Conclusion The method is accurate, rapid and simple with high sensitivity, precision and repeatability, which has been successfully applied as an effective tool for the multicomponent analysis of CHP.
引文
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[21]常炜.HPLC法测定智托洁白丸中木香烃内酯和去氢木香内酯[J].中成药,2011,33(11):1923-1926.
[22]中国药典[S].一部.2010.
[23]中国药典[S].一部.2015.
[2]卫生部颁药品标准(中药成方制剂):第九册[S].1995.
[3]国家中成药标准汇编:内科脾胃分册[S].2002.
[4]徐成志.HPLC法测定沉香化滞丸中大黄素、大黄酚的含量[J].安徽医药,2006,10(12):924-925.
[5]苏瑞林,侯凯,徐华,等.HPLC法测定沉香化滞丸中的大黄酚和大黄素的含量[J].北方药学,2006,3(4):12-14.
[6]郭巧技,肖丽和,熊英.HPLC法测定沉香化滞丸中橙皮苷的含量[J].中国实验方剂学杂志,2009,15(10):32-33.
[7]郭巧技,肖丽和,熊英.沉香化滞丸质量标准研究[J].中国药房,2010,21(7):632-634.
[8]梅全喜,林焕泽,李红念.沉香的药用历史、品种、产地研究应用浅述[J].中国中医药现代远程教育,2013,11(8):85-88.
[9]张玉洁,李和平,张晓珂.沉香化滞丸质量标准研究[J].时珍国医国药,2001,12(8):702-703.
[10]顾宇凡,张倩,霍会霞,等.HPLC-DAD测定沉香药材中沉香四醇的含量[J].世界科学技术-中医药现代化,2014,16(12):2643-2646.
[11]那顺白乙拉,孟和.HPLC法测定清心沉香八味散中沉香四醇的含量[J].中国民族民间医药,2017,26(12):11-13.
[12]宋剑锋,冯敬骞,胡建华,等.HPLC法同时测定常山胡柚花中柚皮苷、橙皮苷和新橙皮苷的量[J].中草药,2014,45(6):854-856.
[13]凌宁生,杨瑾,律兆荣,等.HPLC法测定胃肠安丸中柚皮苷[J].中草药,2005,36(12):1815-1816.
[14]严晓丽,闫倩倩,刘晓政,等.高效液相色谱法测定衢枳壳中新橙皮苷及柚皮苷[J].食品研究与开发,2018,39(21):161-166.
[15]彭玲娜,丁野,孙辉,等.HPLC法同时测定胃痛丸中柚皮苷、新橙皮苷的含量[J].中国药师,2017,20(6):1112-1114.
[16]李松,浦香兰.HPLC-DAD法测定接骨丸中芍药苷、柚皮苷、橙皮苷、丹酚酸B和丹参酮IIA[J].现代药物与临床,2015,30(2):153-156.
[17]王景文,邢晓东.HPLC法测定宁嗽化痰丸中的橙皮苷[J].药物评价研究,2014,37(3):269-271.
[18]刘翔.HPLC法测定麻仁丸中厚朴酚、和厚朴酚、大黄素和大黄酚[J].中草药,2010,41(4):582-583.
[19]蒙毅,范卫锋,钟一雄,等.HPLC法测定红穿破石中大黄素和大黄素甲醚[J].中草药,2007,38(9):1410-1411.
[20]焦正花,刘效栓,杨金草.RP-HPLC测定藏药六味木香丸中木香烃内酯和去氢木香内酯含量[J].中国中医药信息杂志,2015,22(10):94-96.
[21]常炜.HPLC法测定智托洁白丸中木香烃内酯和去氢木香内酯[J].中成药,2011,33(11):1923-1926.
[22]中国药典[S].一部.2010.
[23]中国药典[S].一部.2015.