高效液相色谱-蒸发光散射检测器法测定黄连清胃丸中栀子苷、知母皂苷AⅢ和知母皂苷BⅡ的含量
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摘要
目的:应用高效液相色谱-蒸发光散射检测器(HPLC-ELSD)法测定黄连清胃丸中栀子苷、知母皂苷AⅢ和知母皂苷BⅡ的含量。方法:采用C18色谱柱(4.6 mm×250 mm,5μm);流速为0.9 ml/min;乙腈-水(30∶70)为流动相;ELSD漂移管温度为90℃;载气(N2)流速为2.9 SLPM/min。结果:栀子苷、知母皂苷AⅢ和知母皂苷BⅡ进样量分别在0.061 8~1.236 0μg(r=0.999 2)、0.047 6~0.952 0μg(r=0.999 7)和0.184 2~3.684 0μg(r=0.999 3)时进样量的自然对数值与峰面积的自然对数值呈良好的线性关系,平均加样回收率分别为97.67%、98.18%和98.36%,RSD分别为1.09%、1.01%和0.98%(n=6)。结论:本方法测定结果准确、灵敏、重复性好。
OBJECTIVE: To develop HPLC-ELSD method for determination of the contents of Geniposide, Timosaponin AⅢ and Timosaponin BⅡ in Huanglian Qingwei Pills.METHODS: C 18 column( 4.6 mm × 250 mm, 5 μm) was used as the chromatographic column with mobile phase consisting of Acetonitrile-Water( 30∶ 70) at flow rate of 0.9 ml / min; the temperature of drift tube was set at 90 ℃ and the flow rate of the carrier gas( N 2) was set at 2.9 SLPM / min.RESULTS: The linear ranges of Geniposide,Timosaponin A Ⅲ,Timosaponin B Ⅱ were 0.061 8-1.236 0 μg( r = 0.999 2),0.047 6-0.952 0 μg( r = 0.999 7) and 0.184 2-3.684 0 μg( r = 0.999 3),respectively with average recovery rates of 97.67%( RSD = 1.09%),98.18%( RSD = 1.01%) and 98.3%( RSD = 0.98%), respectively.CONCLUSION: The established method is accurate in determination results,sensitive and reproducible.
OBJECTIVE: To develop HPLC-ELSD method for determination of the contents of Geniposide, Timosaponin AⅢ and Timosaponin BⅡ in Huanglian Qingwei Pills.METHODS: C 18 column( 4.6 mm × 250 mm, 5 μm) was used as the chromatographic column with mobile phase consisting of Acetonitrile-Water( 30∶ 70) at flow rate of 0.9 ml / min; the temperature of drift tube was set at 90 ℃ and the flow rate of the carrier gas( N 2) was set at 2.9 SLPM / min.RESULTS: The linear ranges of Geniposide,Timosaponin A Ⅲ,Timosaponin B Ⅱ were 0.061 8-1.236 0 μg( r = 0.999 2),0.047 6-0.952 0 μg( r = 0.999 7) and 0.184 2-3.684 0 μg( r = 0.999 3),respectively with average recovery rates of 97.67%( RSD = 1.09%),98.18%( RSD = 1.01%) and 98.3%( RSD = 0.98%), respectively.CONCLUSION: The established method is accurate in determination results,sensitive and reproducible.
引文
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[4]聂聪珍.高效液相色谱法测定小儿退热合剂中栀子苷的含量[J].中国医药指南,2013,(14):486-486,487.
[5]邱卓星,熊学敏,胡晓艳,等.HPLC法测定栀子超微速溶饮片中栀子苷的含量[J].中国医药科学,2013,3(3):116-117,127.
[6]李翔,刘皈阳,马建丽,等.HPLC法测定丹膝颗粒中栀子苷的含量[J].中国药师,2013,16(3):468-469.
[7]胡军波,张红萍.HPLC法测定清热解毒胶囊中栀子苷的含量[J].海峡药学,2013,25(2):44-46.
[8]王子雯,唐灿,孙嘉婧,等.多指标综合评判巴中产栀子的采收期和生长期[J].药物分析杂志,2012,32(9):1554-1558,1563.
[9]倪文澎,朱敏,周琴妹.HPLC-ELSD法测定滋肾通关胶囊中2种知母皂苷类成分[J].江苏中医药,2012,44(11):69-70.
[10]王贵金,裴彩云,贾继明,等.HPLC-ELSD法测定周络通胶囊中知母皂苷BⅡ[J].药物评价研究,2011,34(3):187-189.
[11]赵兵,陈千良,倪士峰,等.栽培西陵知母中菝葜皂苷元含量动态研究[J].辽宁中医药大学学报,2011,13(3):22-24.
[12]钟可,王文全,靳风云,等.HPLC-ELSD法同时测定河北产道地药材不同物候期知母中知母皂苷AⅢ和知母皂苷BⅡ的含量[J].中华中医药杂志(原中国医药学报),2013,28(6):1710-1713.
[2]国家药典委员会.中华人民共和国药典:一部[S].2010年版.北京:中国医药科技出版社,2010:197-198,231-232,附录36-附录38.
[3]刘颖,梁洪,祁进,等.龙胆泻肝胶囊及软胶囊质量标准研究[J].中国中医药信息杂志,2013(10):54-58,59.
[4]聂聪珍.高效液相色谱法测定小儿退热合剂中栀子苷的含量[J].中国医药指南,2013,(14):486-486,487.
[5]邱卓星,熊学敏,胡晓艳,等.HPLC法测定栀子超微速溶饮片中栀子苷的含量[J].中国医药科学,2013,3(3):116-117,127.
[6]李翔,刘皈阳,马建丽,等.HPLC法测定丹膝颗粒中栀子苷的含量[J].中国药师,2013,16(3):468-469.
[7]胡军波,张红萍.HPLC法测定清热解毒胶囊中栀子苷的含量[J].海峡药学,2013,25(2):44-46.
[8]王子雯,唐灿,孙嘉婧,等.多指标综合评判巴中产栀子的采收期和生长期[J].药物分析杂志,2012,32(9):1554-1558,1563.
[9]倪文澎,朱敏,周琴妹.HPLC-ELSD法测定滋肾通关胶囊中2种知母皂苷类成分[J].江苏中医药,2012,44(11):69-70.
[10]王贵金,裴彩云,贾继明,等.HPLC-ELSD法测定周络通胶囊中知母皂苷BⅡ[J].药物评价研究,2011,34(3):187-189.
[11]赵兵,陈千良,倪士峰,等.栽培西陵知母中菝葜皂苷元含量动态研究[J].辽宁中医药大学学报,2011,13(3):22-24.
[12]钟可,王文全,靳风云,等.HPLC-ELSD法同时测定河北产道地药材不同物候期知母中知母皂苷AⅢ和知母皂苷BⅡ的含量[J].中华中医药杂志(原中国医药学报),2013,28(6):1710-1713.