HPLC法测定威喜丸中猪苓酮B、猪苓酮A、去氢土莫酸、猪苓酸C、去氢茯苓酸和茯苓酸
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摘要
目的建立HPLC波长切换法同时测定威喜丸中猪苓酮B、猪苓酮A、去氢土莫酸、猪苓酸C、去氢茯苓酸和茯苓酸的方法。方法采用Agilent Eclipse XDB-C18色谱柱(250 mm×4.6 mm,5μm);流动相:乙腈–0.05%磷酸溶液,梯度洗脱;0～24.0 min在248 nm波长下检测猪苓酮B和猪苓酮A,24.0～50.0 min在210 nm波长下检测去氢土莫酸、猪苓酸C、去氢茯苓酸和茯苓酸;体积流量1.0m L/min;柱温30℃;进样量为10μL。结果猪苓酮B、猪苓酮A、去氢土莫酸、猪苓酸C、去氢茯苓酸和茯苓酸分别在5.79～115.80、1.66～33.20、3.28～65.60、7.07～141.40、1.46～29.20、0.88～17.60μg/mL与峰面积线性关系良好;平均加样回收率分别为98.75%、97.60%、98.23%、99.49%、97.10%、96.81%,RSD值分别为0.75%、1.66%、1.44%、0.90%、1.15%、1.38%。结论本方法简便、准确、重复性好,为威喜丸的质量控制提供了实验依据。
Objective To establish an HPLC with wavelength switching method for determination of polyporusterone B, polyporusterone A, dehydrotumulosic acid, polyporenic acid C, dehydropachymic acid, and pachymic acid in Weixi Pills. MethodsThe separation was carried out on Agilent Eclipse XDB-C18 chromatography column(250 mm × 4.6 mm, 5 μm). The mobile phase consisted of acetonitrile-0.05% phosphoric acid solution with gradient elution. The detection wavelengths were set at 248 nm in 0 — 24.0 min(determination of polyporusterone B and polyporusterone A) and 210 nm in 24.0 — 50.0 min(determination of dehydrotumulosic acid, polyporenic acid C, dehydropachymic acid and pachymic acid). The flow rate was 1.0 mL/min, temperature of column was set at 30 ℃, and volume of injection was 10 μL. Results The linear ranges of polyporusterone B, polyporusterone A, dehydrotumulosic acid, polyporenic acid C, dehydropachymic acid, and pachymic acid were 5.79 — 115.80, 1.66 — 33.20, 3.28 — 65.60, 7.07 — 141.40, 1.46 — 29.20, and 0.88 — 17.60 μg/m L, respectively. The average recoveries were 98.75%, 97.60%, 98.23%, 99.49%, 97.10%, and 96.81%, with RSD 0.75%, 1.66%, 1.44%, 0.90%, 1.15%, and 1.38%. Conclusion The method is simple, accurate and reproducible, and provides an experimental basis for the quality control of Weixi Pills.
Objective To establish an HPLC with wavelength switching method for determination of polyporusterone B, polyporusterone A, dehydrotumulosic acid, polyporenic acid C, dehydropachymic acid, and pachymic acid in Weixi Pills. MethodsThe separation was carried out on Agilent Eclipse XDB-C18 chromatography column(250 mm × 4.6 mm, 5 μm). The mobile phase consisted of acetonitrile-0.05% phosphoric acid solution with gradient elution. The detection wavelengths were set at 248 nm in 0 — 24.0 min(determination of polyporusterone B and polyporusterone A) and 210 nm in 24.0 — 50.0 min(determination of dehydrotumulosic acid, polyporenic acid C, dehydropachymic acid and pachymic acid). The flow rate was 1.0 mL/min, temperature of column was set at 30 ℃, and volume of injection was 10 μL. Results The linear ranges of polyporusterone B, polyporusterone A, dehydrotumulosic acid, polyporenic acid C, dehydropachymic acid, and pachymic acid were 5.79 — 115.80, 1.66 — 33.20, 3.28 — 65.60, 7.07 — 141.40, 1.46 — 29.20, and 0.88 — 17.60 μg/m L, respectively. The average recoveries were 98.75%, 97.60%, 98.23%, 99.49%, 97.10%, and 96.81%, with RSD 0.75%, 1.66%, 1.44%, 0.90%, 1.15%, and 1.38%. Conclusion The method is simple, accurate and reproducible, and provides an experimental basis for the quality control of Weixi Pills.
引文
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[6]张靓琦,贾英,罗洁,等.超高效液相色谱法同时测定茯苓中去氢土莫酸等6种活性成分的含量[J].中国药学杂志,2012,47(13):1080-1083.
[7]车爽,李清,霍艳双,等.波长转换RP-HPLC法同时测定茯苓不同部位中5种三萜酸含量[J].药学学报,2010,45(4):494-497.
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[9]沈玉萍,杨欢,陈斌,等.反相高效液相色谱法测定中药茯苓中4种三萜酸的含量[J].中国药学杂志,2011,46(5):388-390.
[10]王弘,晁建平,陈文举,等.猪苓药材的质量评价标准研究[J].中草药,2009,40(6):971-974.
[2]乔铁锤.威喜丸治白带[J].四川中医,1990(3):388-390.
[3]方厚贤,杨容.威喜丸治疗乳糜尿-名医张羹梅临床经验介绍[J].中国冶金工业医学杂志,1990,7(6):260-260.
[4]中国药典[S].一部.2015:240-241,318-319.
[5]陈晓梅,周微微,王春兰,等.猪苓甾酮类化合物的HPLC含量测定及指纹图谱研究[J].菌物学报,2017,36(1):83-97.
[6]张靓琦,贾英,罗洁,等.超高效液相色谱法同时测定茯苓中去氢土莫酸等6种活性成分的含量[J].中国药学杂志,2012,47(13):1080-1083.
[7]车爽,李清,霍艳双,等.波长转换RP-HPLC法同时测定茯苓不同部位中5种三萜酸含量[J].药学学报,2010,45(4):494-497.
[8]谭庆龙,李楚坚,金苗,等.HPLC法同时测定猪苓中6个甾体类成分的含量[J].中药材,2017,40(8):1892-1894.
[9]沈玉萍,杨欢,陈斌,等.反相高效液相色谱法测定中药茯苓中4种三萜酸的含量[J].中国药学杂志,2011,46(5):388-390.
[10]王弘,晁建平,陈文举,等.猪苓药材的质量评价标准研究[J].中草药,2009,40(6):971-974.