基于一测多评法同时定量测定人参女金丸中9个主要成分
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摘要
目的建立一测多评法同时测定人参女金丸中洋川芎内酯H、洋川芎内酯I、洋川芎内酯A、藁本内酯、氧化芍药苷、芍药内酯苷、芍药苷、苯甲酰芍药苷和α-香附酮的含量,为其质量标准的研究提供依据。方法采用Agilent Zorbax SB C18色谱柱(4. 6 mm×250 mm,5μm);以甲醇-乙腈(2∶1)与0. 1%磷酸溶液为流动相,梯度洗脱;流速为0. 9 m L·min-1;柱温30℃;检测波长分别为:280、230和242 nm;以芍药苷为内参物,建立人参女金丸中洋川芎内酯H、洋川芎内酯I、洋川芎内酯A、藁本内酯、氧化芍药苷、芍药内酯苷、苯甲酰芍药苷和α-香附酮与该成分的相对校正因子,通过一测多评法与外标法结果的比较,验证所建立方法的准确性和可行性。结果洋川芎内酯H、洋川芎内酯I、洋川芎内酯A、藁本内酯、氧化芍药苷、芍药内酯苷、芍药苷、苯甲酰芍药苷和α-香附酮在一定范围内浓度与峰面积呈良好的线性关系;精密度、稳定性、重现性等均符合方法学要求;平均加样回收率分别为97. 38%、98. 16%、98. 84%、99. 63%、97. 04%、99. 14%、100. 04%、96. 93%和98. 48%,RSD分别为1. 38%、1. 18%、0. 97%、0. 86%、1. 68%、1. 30%、0. 57%、1. 32%和1. 19%;一测多评法所得结果与外标法结果无显著差异。结论一测多评法可以用于人参女金丸中9个成分的含量测定及质量控制。
OBJECTIVE To establish a quantitative analysis of multi-components by single-marker( QAMS) method for simultaneous determination of senkyunolide H,senkyunolide I,senkyunolide A,ligustilide,oxypaeoniflorin,albiflorin,paeoniflorin,benzoylpaeoniflorin and α-cyperone in Renshen Nüjin pills,in order to provide basis for studying its quality standards. METHODS The analysis of the methanol extract of Renshen Nüjin pills was performed on Agilent Zorbax SB C18 column( 4. 6 mm × 250 mm,5 μm),with mobile phase composed of methanol-acetonitrile( 2∶ 1)-0. 1% phosphoric acid solution at a flow rate of 0. 9 m L·min-1 in gradient elution mode. The column temperature was maintained at 30 ℃,and the detection wavelengths were set at 280,230 and 242 nm. Paeoniflorin was selected as the internal standard,and the relative correlation factors( RCF) of senkyunolide H,senkyunolide I,senkyunolide A,ligustilide,oxypaeoniflorin,albiflorin,paeoniflorin,benzoylpaeoniflorin and α-cyperone were determined by HPLC. The accuracy and feasibility of the method were validated by comparing the results of QAMS method and external standard method.RESULTS The standard curves of senkyunolide H,senkyunolide I,senkyunolide A,ligustilide,oxypaeoniflorin,albiflorin,paeoniflorin,benzoylpaeoniflorin and α-cyperone had good linear relationship in the ranges of the tested concentrations. The precision,stability and repeatability complied with the requirements of methodology. The recoveries were 97. 38%,98. 16%,98. 84%,99. 63%,97. 04%,99. 14%,100. 04%,96. 93% and 98. 48%,RSDs were 1. 38%,1. 18%,0. 97%,0. 86%,1. 68%,1. 30%,0. 57%,1. 32% and 1. 19%,respectively. No significant differences were observed in the determination results by QAMS method and external standard method. CONCLUSION The QAMS method can be used for the content determination and quality control of the nine components in Renshen Nüjin pills.
OBJECTIVE To establish a quantitative analysis of multi-components by single-marker( QAMS) method for simultaneous determination of senkyunolide H,senkyunolide I,senkyunolide A,ligustilide,oxypaeoniflorin,albiflorin,paeoniflorin,benzoylpaeoniflorin and α-cyperone in Renshen Nüjin pills,in order to provide basis for studying its quality standards. METHODS The analysis of the methanol extract of Renshen Nüjin pills was performed on Agilent Zorbax SB C18 column( 4. 6 mm × 250 mm,5 μm),with mobile phase composed of methanol-acetonitrile( 2∶ 1)-0. 1% phosphoric acid solution at a flow rate of 0. 9 m L·min-1 in gradient elution mode. The column temperature was maintained at 30 ℃,and the detection wavelengths were set at 280,230 and 242 nm. Paeoniflorin was selected as the internal standard,and the relative correlation factors( RCF) of senkyunolide H,senkyunolide I,senkyunolide A,ligustilide,oxypaeoniflorin,albiflorin,paeoniflorin,benzoylpaeoniflorin and α-cyperone were determined by HPLC. The accuracy and feasibility of the method were validated by comparing the results of QAMS method and external standard method.RESULTS The standard curves of senkyunolide H,senkyunolide I,senkyunolide A,ligustilide,oxypaeoniflorin,albiflorin,paeoniflorin,benzoylpaeoniflorin and α-cyperone had good linear relationship in the ranges of the tested concentrations. The precision,stability and repeatability complied with the requirements of methodology. The recoveries were 97. 38%,98. 16%,98. 84%,99. 63%,97. 04%,99. 14%,100. 04%,96. 93% and 98. 48%,RSDs were 1. 38%,1. 18%,0. 97%,0. 86%,1. 68%,1. 30%,0. 57%,1. 32% and 1. 19%,respectively. No significant differences were observed in the determination results by QAMS method and external standard method. CONCLUSION The QAMS method can be used for the content determination and quality control of the nine components in Renshen Nüjin pills.
引文
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[14]JI N P,LU J R,LI W B,et al.Influences of different vinegar processing methods on contents of index components in Cyperi Rhizoma[J].Chin J Exp Tradit Med Form(中国实验方剂学杂志),2015,21(7):5-7.
[15]WANG X T,WANG L,SONG D C,et al.Determination ofα-cyperone in Cyperi Rhizoma from various habitats[J].Tianjin Sci Technol(天津科技),2013,22(1):28-29.
[16]LIU J,XU W,LI H,et al.Simultaneous determination of ten components in Radix Paeoniae Alba pieces by UPLC-MS/MS[J].Chin J Pharm Anal(药物分析杂志),2015,35(4):635-643.
[2]Ch.P(2015)Vol I(中国药典2015年版.一部)[S].2015:40,105,133,258.
[3]LI W M,ZHAO Y R,YANG Y Y,et al.RP-HPLC with UVswitch determination of nine components in white Peony Root pieces[J].Chin J Pharm Anal(药物分析杂志),2011,31(12):2208-2212.
[4]YANG Y,PENG F,MO Z C,et al.Determination of five chemical ingredients in Moutan Cortex from various habitats by HPLC[J].J Chin Med Mater(中药材),2011,36(3):416-422.
[5]XU Y,ZHANG W J,WANG Q W,et al.Research on the HPLC fingerprints of different processed Cyperi Rhizoma[J].Chin Med Rep(中国医药导报),2011,8(31):29-32.
[6]CAO J M,WANG Z H,DING M Y,et al.Determination of lactone components in Chuanxiong by reversed-phase high performance liquid chromatography[J].Chin J Chromatogr(色谱),2005,23(5):531-533.
[7]LIU J L,FAN Q J,ZHENG S L,et al.Quantitative determination of five active ingredients in different harvest periods of Ligusticum chuanxiong by HPLC[J].China J Chin Mater Med(中国中药杂志),2014,39(9):1650-1655.
[8]ZHANG L J,LIU J Y,YAO C,et al.Research progress in pharmacological activities of senkyunolides[J].Chin Pharm J(中国药学杂志),2015,50(13):1081-1084.
[9]TIAN L,YAN H X,FU X T,et al.Simultaneous determination of multiple components in decoction pieces of Chuanxiong Rhizoma and Angelicae Sinensis Radix by quantitative analysis of multi-components by single maker[J].Chin J Pharm Anal(药物分析杂志),2014,34(5):848-854.
[10]WANG Z M,GAO H M,HU X T,et al.Multi-components quantitation by onemarker new method for quality evaluation of Chinese herbal medicine[J].China J Chin Mater Med(中国中药杂志),2006,31(23):1925-1928.
[11]YANG Y,LIU Y H,HUANG Z F,et al.Determination of senkyunolide A and ligustilide in Chuanxiong Rhizoma and Angelicae Sinensis Radix by QAMS[J].Chin J Exp Tradit Med Form(中国实验方剂学杂志),2015,21(3):58-62.
[12]HE X J,ZHANG Z Q,WANG J N,et al.HPLC with UVswitch determination of eight indicative components in combination extracts of Persicae Ramulus and Paeoniae Radix Alba[J].Chin J Pharm Anal(药物分析杂志),2013,33(11):1899-1903.
[13]LU J R,LI W B,WANG S Y,et al.Contents comparison of cyperotundone,nootkatone andα-cyperone in Cyperi Rhizoma before and after vinegar processing[J].Chin J Exp Tradit Med Form(中国实验方剂学杂志),2014,20(20):24-27.
[14]JI N P,LU J R,LI W B,et al.Influences of different vinegar processing methods on contents of index components in Cyperi Rhizoma[J].Chin J Exp Tradit Med Form(中国实验方剂学杂志),2015,21(7):5-7.
[15]WANG X T,WANG L,SONG D C,et al.Determination ofα-cyperone in Cyperi Rhizoma from various habitats[J].Tianjin Sci Technol(天津科技),2013,22(1):28-29.
[16]LIU J,XU W,LI H,et al.Simultaneous determination of ten components in Radix Paeoniae Alba pieces by UPLC-MS/MS[J].Chin J Pharm Anal(药物分析杂志),2015,35(4):635-643.