目的 优化并完善清开灵滴丸的质量控制方法。方法 采用高效液相色谱法对清开灵滴丸中的黄芩苷进行鉴别;采用薄层色谱法对清开灵滴丸中金银花及其所含绿原酸、栀子所含栀子苷进行鉴别。采用高效液相色谱法-蒸发光检测器同时测定清开灵滴丸中胆酸和猪去氧胆酸的含量,色谱柱为Phenomenex Gemini 110 C18 (4.6 mm×250 mm, 5 μm),流动相为甲醇-乙腈-0.1%甲酸(68∶17∶15),流速为1.0 mL·min-1。采用高效液相色谱法测定清开灵滴丸中栀子苷的含量,色谱柱为Agilent Eclipse XDB-C18(4.6 mm×150 mm,5 μm);流动相为乙腈-0.05%磷酸(10∶90),流速为1.0 mL·min-1;检测波长为238 nm。采用高效液相色谱法测定清开灵滴丸中黄芩苷的含量,色谱柱为同栀子苷含量测定;流动相为甲醇-水-磷酸(47∶53∶0.2),流速为1.0 mL·min-1;检测波长为275 nm。结果 薄层色谱斑点清晰,重现性好。猪去氧胆酸、胆酸、栀子苷和黄芩苷进样量分别在0.505 0～6.312 μg、0.515～6.440 μg、0.029 12～0.582 4 μg和0.109 2～1.092 μg内与峰面积(或峰面积对数)呈良好线性关系,平均回收率分别为101.5%、101.6%、98.61%和99.77%,RSD分别为1.7%、1.5%、1.42%和0.79%。结论 提高后的质量标准分析方法简便、快速、准确且毒性较小,能更全面有效控制清开灵滴丸的质量。
Abstract
OBJECTIVE To optimize and improve the quality standard of Qingkailing dropping pills. METHODS Lonicerae Japonicae Flos, geniposide in Gardeniae Fructus and baicalin in Scutellariae Radix of Qingkailing dropping pills were identified by TLC and HPLC respectively. Cholic acid and hydrodeoxycholic acid were determined by HPLC equipped with an ELSD and a column (4.6 mm×250 mm, 5 μm) packed with ODS bonded silica gel (5 μm particle size). The mobile phase was a mixture of methanol, acetonitrile and 0.1% formic acid (68∶17∶15, V/V/V) and the flow rate was 1.0 mL·min-1. Geniposide in Gardeniae Fructus of Qingkailing dropping pills was determined by HPLC equipped with a DAD (238 nm) and a column (4.6 mm×250 mm) packed with ODS bonded silica gel (5 μm particle size). The mobile phase was a mixture of acetonitrile and 0.05% phosphoric acid (10∶90, V/V) and the flow rate was 1.0 mL·min-1. Baicalin in Scutellariae Radix of Qingkailing dropping pills was determined by HPLC equipped with a DAD (275 nm) and a column (4.6 mm×150 mm) packed with ODS bonded silica gel (5 μm particle size), the mobile phase was a mixture of methnol, water and phosphoric acid (47∶53∶0.2, V/V/V), and the flow rate was 1.0 mL·min-1. RESULTS The developed TLC spots were clear with good reproducibility. Hydrodeoxycholic acid, cholic acid, geniposide and baicalin showed good linear relationship in the ranges of 0.505 0-6.312 μg, 0.515-6.440 μg, 0.029 12-0.582 4 μg, and 0.109 2-1.092 μg, respectively. The average recoveries (n=6) were 101.5%, 101.6%, 98.61% and 99.77%, with RSDs of 1.7%, 1.5%, 1.42% and 0.79%, respectively. CONCLUSION The method is simple, rapid, accurate, with low toxicity, and can be used to control the quality of Qingkailing dropping pills more effectively and comprehensively.
关键词
清开灵滴丸 /
胆酸 /
猪去氧胆酸 /
金银花 /
栀子苷 /
黄芩苷 /
薄层色谱 /
高效液相色谱法
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Key words
Qingkailing dropping pills /
cholic acid /
hydrodeoxycholic acid /
Lonicerae Japonicae Flos /
geniposide /
baicalin /
TLC /
HPLC
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中图分类号：
R917
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参考文献
[1] National drug standards new drug standardization (国家药品标准新药转正标准). Vol 33 [S]. 2010:77-79.
[2] National drug standards(国家药品标准). WS3-123(Z-123)-2001(Z)-1[S]. 2015: 1-5.
[3] National drug standards(国家药品标准) . WS3-123(Z-123)-2001(Z)-2[S]. 2015: 1-5.
[4] CHEN W J, TENG Q, WANG C Y. Determination of cholaic acid and hyodeoxycholic acid in Qingkailing Diwan by HPLC-ELSD [J]. J Huaiyin Teach Coll(Nat Sci Ed)(淮阴师范学院学报:自然科学版), 2013, 12(3):236-239.
[5] XU X L, SHI X. Determination of cholaic acid in Qingkailing Diwan by HPLC method [J]. China Pharm(中国药师), 2010, 13(12):1828-1829.
[6] GAO M. Content determination of hyodeoxycholic acid in Qingkailing Diwan by HPLC method [J]. Harbin Med J(哈尔滨医药), 2008, (4):45-46.
[7] LI G B, LIU S S, LI Z G. Simultaneous determination of cholaic acid and hyodeoxycholic acid in Qingkailing Zhusheye by HPLC-ELSD [J]. Tradit Chin Med Res(中医研究), 2013, 26(11):72-75.
[8] WANG L, DAI J, NIU X L. HPLC-ELSD Determination of cholic acid and hydrodeoxycholic acid contents in Qingkailing Soft Capsule [J]. China Pharm(中国药业), 2013, 22(12):79-80.
[9] YANG L W, LIU X X, GONG J, et al. Universal method for the determination of cholic acid and hydrodeoxycholic acid in Qingkailing Preparations [J]. J China Pharm(中国药房), 2012, 23(35):3340-3342.
[10] BI X Y, LIU X F, HU P, et al. Determination of cholic acid and geniposide in Qingkailing Tablets by HPLC [J]. Lishizhen Med Mater Med Res(时珍国医国药), 2012, 23(3):663-665.
[11] HAN J. Determination of four active components in Qingkailing Granules by HPLC [J]. Chin Tradit Pat Med(中成药), 2010, 32(2):227-231.
[12] WANG Q, CAO J, LIU J X, et al. HPLC Specific chromatogram of Qingkailing Injection and its application in quality control [J]. Chin J Pharm Anal(药物分析杂志), 2010, 30(1):37-40.
[13] WANG W J, JIA X D, XIAO Y, et al. Content determination of geniposide in Qingkailing Diwan by HPLC [J]. China J Chin Mater Med(中国中药杂志), 2005(13):1034-1035.
[14] HU Y N. Content determination research of geniposide in Qingkailing Diwan by HPLC [J]. China Pract Med(中国实用医药), 2014, 9(2):252-253.
[15] LIU F, HUANG X H, FU M Q, et al. Content determination of geniposide in compound Qingkailing Injection by HPLC [J]. J South China Agricultural Univ(华南农业大学学报), 2010, 31(4):104-107.
[16] Ch.P (2015) VolⅠ(中国药典2015年版.一部) [S]. 2015:1529-1531.
[17] SHI Y H. Determination of geniposide and baicalin in Qingkailing Capsule by dual-wavelength RP-HPLC [J]. Pract Pharm Clin Remed(实用药物与临床), 2011, 14(4):300-303.
[18] LI L L, ZHAO L F. Determination of baicalin for different preparations of Qingkailing [J]. Chin J Pharm Anal(药物分析杂志), 2011, 31(5):950-953.
[19] ZHANG Y, LI Z H. Content determination of baicalin in Qingkailing Keli by HPLC method [J]. Hubei J Tradit Chin Med(湖北中医杂志), 2011, 33(7):79-80.
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脚注
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基金
国家药品标准提高暨2020年版药典科研项目资助
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