波长切换HPLC法同时测定六神曲中9个成分的含量
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摘要
目的:建立波长切换HPLC法同时测定六神曲中苦杏仁苷、青蒿素、香草酸、芦丁、金丝桃苷、阿魏酸、槲皮苷、槲皮素、山柰酚共9个成分的含量。方法:采用Agela Venusil XBP C18(2)硅胶色谱柱(4.6mm×250 mm,5μm),以乙腈为流动相A,0.08%磷酸水溶液为流动相B,梯度洗脱,流速为1 mL·min~(-1),柱温为30℃,波长切换(0～15 min,46～62 min,210 nm,检测苦杏仁苷、青蒿素;15～24.9 min,27～46 min,258 nm,检测香草酸、芦丁、金丝桃苷、槲皮苷、槲皮素、山柰酚;24.9～27 min,218 nm,检测阿魏酸)。结果:在上述条件下,1次进样可同时测定9个成分。苦杏仁苷、青蒿素、香草酸、芦丁、金丝桃苷、阿魏酸、槲皮苷、槲皮素、山柰酚的进样量分别在31.95～639μg(r=0.999 5),595～11 900μg(r=0.999 4),17.82～356.32μg(r=0.999 9),17.27～345.44μg(r=0.999 9),20.88～417.60μg(r=0.999 9),75.6～1 512μg(r=0.999 9),15.93～318.50μg(r=0.999 9),8.7～174μg(r=0.999 8),13.2～264μg(r=0.999 9)范围内与峰面积呈良好线性关系;平均加样回收率(n=6)均高于95.0%,RSD均小于3.0%。10批样品中,上述9个成分含量测定结果依次为9.720～57.265、0～554.585、2.223～32.172、1.790～26.464、1.395～34.503、14.433～82.195、0.265～16.167、0.133～7.463、0.866～5.433μg·g~(-1)。结论:该方法简便,测定结果准确,可用于六神曲的质量控制。
Objective:To establish a method of simultaneous determination of amygdalin,artemisinin,vanillic acid,rutin,hyperoside,ferulic acid,quercitrin,quercetin and kaempferol in Massa Medicata Fermentata by HPLC with wavelength switching. Methods:Agela Venusil XBP C18(2)(4.6 mm×250 mm,5 μm)was chosen,and gradient elution was conducted with acetonitrile as mobile phase A and 0.08% phosphoric acid as mobile phase B.The flow rate was 1.0 mL·min~(-1) and the column temperature was 30 ℃. The detection wavelength was set at 210 nm for Amygdalin and artemisinin during 0-15 min and 46-62 min,258 nm for vanillic acid,rutin,hyperoside,quercitrin,quercetin and kaempferol during 15-24.9 min and 27-46 min,218 nm for ferulic acid during 24.9-27 min. Results:The linear ranges of amygdalin,artemisinin,vanillic acid,rutin,hyperoside,ferulic acid,quercitrin,quercetin and kaempferol were 31.95-639 μg(r=0.999 5),595-11 900 μg(r=0.999 4),17.82-356.32 μg(r=0.999 9),17.27-345.44 μg(r=0.999 9),20.88-417.60 μg(r=0.999 9),75.6-1 512 μg(r=0.999 9),15.93-318.50 μg(r=0.999 9),8.7-174 μg(r=0.999 8)and 13.2-264 μg(r=0.999 9),respectively. The average recoveries(n=6)were above more than 95.0% with RSD less than 3.0%. The content ranges of ten batches of pilot samples were 9.720-57.265,0-554.585,2.223-32.172,1.790-26.464,1.395-34.503,14.433-82.195,0.265-16.167,0.133-7.463 and 0.866-5.433 μg·g~(-1),respectively.Conclusion:The method is simple and accurate,and can be used for the quality control of Massa Medicata Fermentata.
Objective:To establish a method of simultaneous determination of amygdalin,artemisinin,vanillic acid,rutin,hyperoside,ferulic acid,quercitrin,quercetin and kaempferol in Massa Medicata Fermentata by HPLC with wavelength switching. Methods:Agela Venusil XBP C18(2)(4.6 mm×250 mm,5 μm)was chosen,and gradient elution was conducted with acetonitrile as mobile phase A and 0.08% phosphoric acid as mobile phase B.The flow rate was 1.0 mL·min~(-1) and the column temperature was 30 ℃. The detection wavelength was set at 210 nm for Amygdalin and artemisinin during 0-15 min and 46-62 min,258 nm for vanillic acid,rutin,hyperoside,quercitrin,quercetin and kaempferol during 15-24.9 min and 27-46 min,218 nm for ferulic acid during 24.9-27 min. Results:The linear ranges of amygdalin,artemisinin,vanillic acid,rutin,hyperoside,ferulic acid,quercitrin,quercetin and kaempferol were 31.95-639 μg(r=0.999 5),595-11 900 μg(r=0.999 4),17.82-356.32 μg(r=0.999 9),17.27-345.44 μg(r=0.999 9),20.88-417.60 μg(r=0.999 9),75.6-1 512 μg(r=0.999 9),15.93-318.50 μg(r=0.999 9),8.7-174 μg(r=0.999 8)and 13.2-264 μg(r=0.999 9),respectively. The average recoveries(n=6)were above more than 95.0% with RSD less than 3.0%. The content ranges of ten batches of pilot samples were 9.720-57.265,0-554.585,2.223-32.172,1.790-26.464,1.395-34.503,14.433-82.195,0.265-16.167,0.133-7.463 and 0.866-5.433 μg·g~(-1),respectively.Conclusion:The method is simple and accurate,and can be used for the quality control of Massa Medicata Fermentata.
引文
[1]中华人民共和国药典2015年版.四部[S].2015:419ChP 2015.VolⅣ[S].2015:419
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[4]任巧玲,宋潇潇.六神曲的质量情况分析[J].中国现代药物应用,2010,4(10):113REN QL,SONG XX.Analysis of the quality of Massa Medicata Fermentata[J].Chin J Mod Drug Appl,2010,4(10):113
[5]王彬辉,章文红,张晓芬,等.苦杏仁苷提取工艺及药理作用研究新进展[J].中华中医药学刊,2014,32(2):381WANG BH,ZHANG WH,ZHANG XF,et al.New research progress on extraction process and harmacological effects of amygdalin[J].Chin Arch Tradit Chin Med,2014,32(2):381
[6]刘冲,刘荫贞,乐智勇,等.高效液相色谱-蒸发光散射检测器法测定六神曲中青蒿素的含量[J].中南药学,2017,15(2):225LIU C,LIU YZ,LE ZY,et al.HPLC-ELSD determination of artemisinin in Liushenqu[J].Cent South Pharm,2017,15(2):225
[7]陈静,陈铭阳,孙宇峰,等.六神曲中辣蓼的本草考证[J].中国现代中药,2017,19(1):116CHEN J,CHEN MY,SUN YF,et al.Herbal textual of Laliao in Liushenqu[J].Mod Chin Med,2017,19(1):116
[8]何立美,陈玉婷,刘洪梅,等.高效液相色谱法同时测定水辣蓼提取物中6种黄酮成分的含量[J].广东农业科学,2014,13:94HE LM,CHEN YT,LIU HM,et al.Simultaneous determination of six kinds of flavonoid in extract of Polygonum hydropiper L.by HPLC[J].Guangdong Agric Sci,2014,13:94
[9]刘娟秀,罗益远,刘训红,等.不同采收期苍耳草中酚酸类及蒽醌类成分的动态积累分析[J].中草药,2016,47(7):1204LIU JX,LUO YY,LIU XH,et al.Dynamic changes of phenolic acids and anthraquinones in aerial parts of Xanthium sibiricum from different collection periods[J].Chin Tradit Herb Drugs,2016,47(7):1204
[10]付小梅,刘德鸿,孙艳朝,等.蒙古苍耳草化学成分研究[J].中药材,2016,39(6):1308FU XM,LIU DH,SUN YC,et al.Chemical constituents from Xanthium mongolicum[J].J Chin Med Mater,2016,39(6):1308
[11]谢彦博,徐云,孙盛,等.HPLC测定六神曲中青蒿素、芦丁和槲皮素含量[J].中国酿造,2014,33(10):140XIE YB,XU Y,SUN S,et al.Determination of artemisinin,rutin and quercetin in Massa Medicata Fermentata by HPLC[J].China Bre,2014,33(10):140
[12]王丽芳,高文远,徐鑫,等.鲜干品组方六神曲发酵前后指标成分的LC-MS测定及指纹图谱分析[J].中国实验方剂学杂志,2017,24(1):8WANG LF,GAO WY,XU X,et al.Determination of index components and fingerprint about medicated leaven composed of fresh or dry medicines before and after fermentation by LC-MS[J].Chin J Exp Tradit Med Form,2017,24(1):8
[13]马维维,戚岑聪,张艳聪,等.六神曲固态协同发酵工艺优化及物质动态变化研究[J].中华中医药学刊,2017,35(5):1290MA WW,QI CC,ZHANG YC,et al.Optimization of medicated leaven Solid-state fermentation process and research of material change in the process[J].Chin Arch Tradit Chin Med,2017,35(5):1290
[14]练晶军.六神曲质量特征及发酵变化研究[D].北京:北京中医药大学,2011LIAN JJ.Study on the Quality Characteristics and Fermentation Changes of Massa Medicata Fermentata[D].Beijing:Beijing University of Chinese Medicine,2011
[15]唐亮,谭淑珍,华坤鹏,等.RH-HPLC法测定青蒿素中脱氢青蒿素及9-表-青蒿素的含量[J].湖南文理学院学报(自然科学版),2016,28(1):24TANG L,TAN SZ,HUA KP,et al.Determination of artemisitene and9-epi-artemisinin in artemisinin raw material by RH-HPLC[J].JHunan Univ Arts Sci(Sci Technol),2016,28(1):24
[2]张鹏,陈冰,李宝银,等.六神曲的质量调查与评价研究[J].北京中医药,2017,36(7):658ZHANG P,CHEN B,LI BY,et al.The quality investigation and evaluation of Massa Medicata Fermentata[J].Beijing J Tradit Chin Med,2017,36(7):658
[3]刘振启,刘杰.道地“六神曲”的工艺与混乱品的鉴别[J].首都医药,2009,16(1):40LIU ZQ,LIU J.The production process of chinese drugs of Massa Medicata Fermentata and the identification of chaos[J].Cap Med,2009,16(1):40
[4]任巧玲,宋潇潇.六神曲的质量情况分析[J].中国现代药物应用,2010,4(10):113REN QL,SONG XX.Analysis of the quality of Massa Medicata Fermentata[J].Chin J Mod Drug Appl,2010,4(10):113
[5]王彬辉,章文红,张晓芬,等.苦杏仁苷提取工艺及药理作用研究新进展[J].中华中医药学刊,2014,32(2):381WANG BH,ZHANG WH,ZHANG XF,et al.New research progress on extraction process and harmacological effects of amygdalin[J].Chin Arch Tradit Chin Med,2014,32(2):381
[6]刘冲,刘荫贞,乐智勇,等.高效液相色谱-蒸发光散射检测器法测定六神曲中青蒿素的含量[J].中南药学,2017,15(2):225LIU C,LIU YZ,LE ZY,et al.HPLC-ELSD determination of artemisinin in Liushenqu[J].Cent South Pharm,2017,15(2):225
[7]陈静,陈铭阳,孙宇峰,等.六神曲中辣蓼的本草考证[J].中国现代中药,2017,19(1):116CHEN J,CHEN MY,SUN YF,et al.Herbal textual of Laliao in Liushenqu[J].Mod Chin Med,2017,19(1):116
[8]何立美,陈玉婷,刘洪梅,等.高效液相色谱法同时测定水辣蓼提取物中6种黄酮成分的含量[J].广东农业科学,2014,13:94HE LM,CHEN YT,LIU HM,et al.Simultaneous determination of six kinds of flavonoid in extract of Polygonum hydropiper L.by HPLC[J].Guangdong Agric Sci,2014,13:94
[9]刘娟秀,罗益远,刘训红,等.不同采收期苍耳草中酚酸类及蒽醌类成分的动态积累分析[J].中草药,2016,47(7):1204LIU JX,LUO YY,LIU XH,et al.Dynamic changes of phenolic acids and anthraquinones in aerial parts of Xanthium sibiricum from different collection periods[J].Chin Tradit Herb Drugs,2016,47(7):1204
[10]付小梅,刘德鸿,孙艳朝,等.蒙古苍耳草化学成分研究[J].中药材,2016,39(6):1308FU XM,LIU DH,SUN YC,et al.Chemical constituents from Xanthium mongolicum[J].J Chin Med Mater,2016,39(6):1308
[11]谢彦博,徐云,孙盛,等.HPLC测定六神曲中青蒿素、芦丁和槲皮素含量[J].中国酿造,2014,33(10):140XIE YB,XU Y,SUN S,et al.Determination of artemisinin,rutin and quercetin in Massa Medicata Fermentata by HPLC[J].China Bre,2014,33(10):140
[12]王丽芳,高文远,徐鑫,等.鲜干品组方六神曲发酵前后指标成分的LC-MS测定及指纹图谱分析[J].中国实验方剂学杂志,2017,24(1):8WANG LF,GAO WY,XU X,et al.Determination of index components and fingerprint about medicated leaven composed of fresh or dry medicines before and after fermentation by LC-MS[J].Chin J Exp Tradit Med Form,2017,24(1):8
[13]马维维,戚岑聪,张艳聪,等.六神曲固态协同发酵工艺优化及物质动态变化研究[J].中华中医药学刊,2017,35(5):1290MA WW,QI CC,ZHANG YC,et al.Optimization of medicated leaven Solid-state fermentation process and research of material change in the process[J].Chin Arch Tradit Chin Med,2017,35(5):1290
[14]练晶军.六神曲质量特征及发酵变化研究[D].北京:北京中医药大学,2011LIAN JJ.Study on the Quality Characteristics and Fermentation Changes of Massa Medicata Fermentata[D].Beijing:Beijing University of Chinese Medicine,2011
[15]唐亮,谭淑珍,华坤鹏,等.RH-HPLC法测定青蒿素中脱氢青蒿素及9-表-青蒿素的含量[J].湖南文理学院学报(自然科学版),2016,28(1):24TANG L,TAN SZ,HUA KP,et al.Determination of artemisitene and9-epi-artemisinin in artemisinin raw material by RH-HPLC[J].JHunan Univ Arts Sci(Sci Technol),2016,28(1):24
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