目的 建立高效液相色谱-电喷雾检测器方法(HPLC-CAD)同时测定芪蛭通络胶囊中人参皂苷Rb1和黄芪甲苷的含量。方法 采用色谱柱为Waters XSclectHss T3-C18(4. 6 mm×250 mm,5 μm),水(A)-乙腈(B)为流动相,梯度洗脱(0 min,15% B;0～10 min,15%~25%B;10～15 min,25%B~31%B;20～50 min,31%B),流速1 mL·min- 1,柱温25 ℃,进样量为20 μL。电喷雾检测器(CAD)雾化器温度为35 ℃,功能参数(power function,PF)为1.0。结果 芪蛭通络胶囊中人参皂苷Rb1和黄芪甲苷均具有良好的线性关系(r＞0.999 0),定量限(LOQ)分别为0.013和0.015 μg,精密度、重复性、24 h稳定性实验的相对标准偏差(RSD)值均小于3.0%,平均加样回收率分别为91.74%和100.09%。结论 本研究建立的HPLC-CAD法可同时对芪蛭通络胶囊中人参皂苷Rb1和黄芪甲苷进行含量测定,为芪蛭通络胶囊的检测分析和质量控制提供了新的方法。
Abstract
OBJECTIVE To develop a HPLC-CAD method for simultaneous determination of ginsenoside Rb1 and astragaloside Ⅳ in Qizhitongluo Capsules. METHODS HPLC analysis was performed on a WatersXSclectHss T3-C18 column (4.6 mm×150 mm, 5 μm), with mobile phase consisting of water solution (A) -acetonitrile (B) at a flow rate of 1.0 mL· min-1 (0 min, 15% B; 0-10 min, 15%-25%B; 10-15 min, 25%-31%B; 20-50 min,31%B),and column temperature was 25 ℃.The injection volume was 20 μL. The nebulizer chamber temperature for the CAD system was maintained at 35 ℃ and the power function (PF) was 1.0. RESULTS The HPLC-CAD approach developed showed good linearity for ginsenoside Rb1 and astragaloside Ⅳ, and the correlation coefficients for calibration curves were both more than 0.9990. The limits of quantitation (LOQ) were found to be 0.013 and 0.015 μg, respectively. The RSDs of precision, repeatability, stability in 24 h were all less than 3.0%. The average recovery rates of ginsenoside Rb1 and astragaloside Ⅳ were 91.74% and 100.09%, respectively. CONCLUSION The established HPLC-CAD method can simultaneously determine ginsenoside Rb1 and astragaloside Ⅳ in Qizhitongluo capsules, which provides a new approach for the analysis and quality control of Qizhitongluo capsules.
关键词
芪蛭通络胶囊 /
高效液相色谱-电喷雾检测器方法 /
人参皂苷Rb1 /
黄芪甲苷 /
含量测定 /
质量控制 /
电喷雾检测器
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Key words
Qizhitongluo capsule /
HPLC-CAD /
ginsenoside Rb1 /
astragaloside Ⅳ /
quantitative determination /
quality control /
charged aerosol detector
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中图分类号：
R284
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参考文献
[1] WANG Y,YU H L,GUO L P. Primary discussion of the keys on the modernization of Chinese medicine[J]. World J Integr Tradit West Med(世界中西医结合杂志), 2014,9(7):768-770.
[2] ZHANG W Z. Study on pharmacodynamics of Tongluocapsules and prescribing drugs in Qizhitongluo capsules based on serum[D].Taiyuan: Shanxi Provincial Institute of Traditional Chinese Medicine, 2020.
[3] WU X W. Preliminary study on pharmacodynamics and serum pharmacology of blood-activating and stasis-resolving drugs in Qizhitongluocapsule[D]. Taiyuan: Shanxi Provincial Institute of Traditional Chinese Medicine, 2019.
[4] LI X Y, JIANG Y B, MA Y Y, et al. The advantages and application progress of electrospray detector in drug HPLC analysis[J]. J China Pharm (中国药房), 2017, 28(15): 2152-2156.
[5] XU D D, DU N N, GENG Y X, et al. Determination of five saponins in 70% ethanol elution effective fraction of Chaihuplus Longgumulidecoction by HPLC-ELSD[J]. Chin Pharm J (中国药学杂志), 2017, 52(10): 861-864.
[6] YING H M, QI Z J, GUO D W, et al. Quantiative determination capolliposide B and in Lysimachia capillipes by HPLC-ELSD assay[J].Chin Pharm J (中国药学杂志),2011, 46(9): 704-706.
[7] SI L T, NI H F, LI Q, et al.Simultaneous determination of five saponins in Yaobitong capsule by HPLC-CAD[J].Acta Pharm Sin (药学学报),2020,55(10):2449-2453.
[8] LIAO Q, WANG L L, WEI R W. Determination of astragaloside Ⅳ in four kinds of chinese patent medicines by ASE-CAD combined with column post compensation liquid chromatography[J].Chin Pharm J (中国药学杂志),2018,53(6):456-459.
[9] ZHOU Z, MIN J G, WU M J, et al. Determination of two isomers asiaticoside B and madecassoside in Sanjintablets by HPLC-CAD[J].Chin Tradit Herb Drugs (中草药),2021,52(14):4217-4220.
[10] LIAO Y, WANG H Y.Determination of the contents of saikosaponin a, b2 and d in bupleurumchinense from different babitats by HPLC-CAD[J]. J Sichuan Tradit Chin Med (四川中医),2020,38(1):62-66.
[11] ZHANG S H, WANG J H, GUO H Z, et al. Determination of fructose,glucose and sucrose in ImperataeRhizoma by HPLC-CAD[J].Chin J Pharm Anal (药物分析杂志),2018,38(6):942-947.
[12] ZHANG X, LI Z, ZHANG Y T, et al. Simultaneous quantification of monosaccharides and disaccharides in RhizomaBletillae by HPLC-CAD[J].J Int Pharm Res (国际药学研究杂志),2018,45(2):154-157.
[13] DENG Y, ZHANG J K, ZONG K, et al.Comparative analysis of carbohydrates in wild and commercial honey by using TLC and HPLC-CAD[J].Chin J Pharm Anal (药物分析杂志),2018,38(1): 22-28.
[14] Ch.P(2020) VolⅣ(中国药典2020年版.四部) [S]. 2020: 8.
[15] GAO H T, HUANG P, LIU J L, et al. Content determination of astragaloside in GuiPipills by HPLC -CAD[J]. Guangzhou Chem Ind(广州化工), 2017, 45(17): 114-116.
[16] REN M, XU Z Z. Determination of six components in Rupixiaogranule by HPLC-ELSD[J]. Liaoning J Tradit Chin Med (辽宁中医杂志),2016,43(1):118-121.
[17] ZHANG X. Research progress on the content determination of astragaloside in astragalusmenmbranaceus[J].Agric Sci Technol Equip (农业科技与装备), 2019,(4): 55-56,59.
[18] CAO W, XU D L, FAN X J, et al.Quantitative determination of ginsenoside Re in Shengmaiyin by HPLC-ELSD method[J].Pharm Care Res (药学服务与研究), 2010,10(3):228-229.
[19] WANG F Y, WU D, ZHAO F M, et al.Determination of astragaloside in Xiaoshuangranules by HPLC[J].Chin J Ethnomed Ethnopharm(中国民族民间医药),2021,30(1):31-33.
[20] ZHAO L, WANG L H, LI W J, et al. Determination of astragalosideⅣ in Yiqibuxuetables by HPLC-ELSD[J].Chin J Drug Eval(中国药物评价),2020,37(6):451-454.
[21] KONG X L, LV Q, LI Y L, et al.Advances in research on pharmacological effect of astragalosideⅣoncardiovascular and cerebrovascular diseases[J].Chin J Exp Tradit Med Form(中国实验方剂学杂志),2021,27(2):218-223.
[22] YU M, GUO S L, YANG K J, et al. Research progress on radix astragali and its preparations in treating heart failure[J].Acta Chin Med Pharm(中医药学报),2021,49(6):94-99.
[23] HUANG S Q. Effects of astragaloside Ⅳ and ferulic acid composition on atherosclerosis in ApoE-/- mice[J].China J Tradit Chin Med Pharm(中华中医药杂志),2021,36(6):3251-3255.
[24] YE H F, ZHANG J, LIU H, et al. Preparation, intracellular distribution and anti-cardiomyocyte apoptosis of astragalosideⅣPEG-PEnanomicelles[J]. Chin Pharm J (中国药学杂志), 2021, 56(10): 815-821.
[25] SHI H,ZHOU P,GAO G,et al. Astragaloside Ⅳ prevents acute myocardial infarction by inhibiting the TLR4/MyD88/NF-κB signaling pathway[J]. J Food Biochem,2021:45(7):doi:0.1111/jfbc.13757
[26] WANG T S. Chineseginseng(中国人参)[M].Shenyang:Liaoning Science and Technology Publishing House,1992.
[27] LUO L M, SHI Y N, JIANG Y N, et al. Advance in components with antitumor effect of Panax ginseng and their mechanisms [J].Chin Tradit Herb Drugs (中草药),2017,48(3):582-596.
[28] CHEN W X, YANG M, YU D W, et al. Hypoglycemic effect and mechanism of the ginseng glycopeptide in diabetic rats with QI and Yin deficiency[J]. Chin Pharm J (中国药学杂志), 2014, 49(21): 1903-1907.
[29] CHEN W M, JIAN M H, ZHAO Y S, et al. Effect of ginsenoside Rg3 on NF-κBp65 and its related inflammatory factors after carotid balloon injury in rats[J]. Chin Pharm J (中国药学杂志), 2018, 53(21): 1831-1835.
[30] ZHANG M, QIN K M, LI W D, et al. Study on chemical constituents change and mechanism of ginseng during processing[J].China J Chin Mater Med(中国中药杂志),2014,39(19):3701-3706.
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