RP-HPLC法同时测定醋延胡索配方颗粒中7种生物碱
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摘要
目的建立RP-HPLC法同时测定醋延胡索配方颗粒中原阿片碱、盐酸巴马汀、盐酸小檗碱、脱氢紫堇碱、延胡索乙素、四氢小檗碱和延胡索甲素的方法。方法采用Ultimate AQ-C18色谱柱(250 mm×4.6 mm,5μm);乙腈-0.1%磷酸水溶液(三乙胺调p H值至6.0)(10∶90)为流动相,梯度洗脱,体积流量为1.0 m L/min,检测波长为280 nm。结果原阿片碱线性范围为6.8~119.0 ng,r=0.999 9,平均回收率为98.2%,RSD为2.0%;盐酸巴马汀线性范围为24.38~426.65 ng,r=0.999 9,平均回收率为99.6%,RSD为2.8%;盐酸小檗碱线性范围为8.88~155.40 ng,r=0.999 9,平均回收率为100.2%,RSD为1.3%;脱氢紫堇碱线性范围为77.66~1 359.05 ng,r=0.999 9,平均回收率为99.0%,RSD为2.2%;延胡索乙素线性范围为41.4~724.5 ng,r=0.999 9,平均回收率为100.8%,RSD为2.6%;四氢小檗碱线性范围为6.70~117.25 ng,r=0.999 7,平均回收率为98.7%,RSD为2.5%;延胡索甲素线性范围为25.50~446.25 ng,r=0.999 9,平均回收率为97.7%,RSD为2.2%。结论该法分离度好,快速简便,重现性好,可用于醋延胡索配方颗粒的质量控制。
Objective To establish HPLC method for the simultaneous determination of protopine, palmatine hydrochloride, berberine hydrochloride, dehydrocorydaline, tetrahydropalmatine, tetrahydroberberine, and corydaline in Cuyanhusuo Granule. Methods The analysis was performed on Ultimate AQ-C18 column(250 mm × 4.6 mm, 5 μm) by gradient elution of acetonitrile-0.1% phosphoric acid(adjust to p H 6.0 with triethylamine)(10︰90). The UV detection wavelength was set at 280 nm and the flow rate was 1.0 m L/min. Results The linear ranges of protopine, palmatine hydrochloride, berberine hydrochloride, dehydrocorydaline, tetrahydropalmatine, tetrahydroberberine, and corydaline were 6.8—119.0(r = 0.999 9), 24.38—426.65(r = 0.999 9), 8.88—155.40(r = 0.999 9), 77.66—1 359.05(r = 0.999 9), 41.4—724.5(r = 0.999 9), 6.70—117.25(r = 0.999 9), and 25.50—446.25 ng(r = 0.999 9). The average recoveries(n = 6) were 98.2%(RSD = 2.0%), 99.6%(RSD = 2.8%), 100.2%(RSD = 1.3%), 99.0%(RSD = 2.2%), 100.8%(RSD = 2.6%), 98.7%(RSD = 2.5%), and 97.7%(RSD = 2.2%), respectively. Conclusion This method is simple and rapid, and can be used for the quality control of Cuyanhusuo Granule with satisfactory separation and repeatability.
Objective To establish HPLC method for the simultaneous determination of protopine, palmatine hydrochloride, berberine hydrochloride, dehydrocorydaline, tetrahydropalmatine, tetrahydroberberine, and corydaline in Cuyanhusuo Granule. Methods The analysis was performed on Ultimate AQ-C18 column(250 mm × 4.6 mm, 5 μm) by gradient elution of acetonitrile-0.1% phosphoric acid(adjust to p H 6.0 with triethylamine)(10︰90). The UV detection wavelength was set at 280 nm and the flow rate was 1.0 m L/min. Results The linear ranges of protopine, palmatine hydrochloride, berberine hydrochloride, dehydrocorydaline, tetrahydropalmatine, tetrahydroberberine, and corydaline were 6.8—119.0(r = 0.999 9), 24.38—426.65(r = 0.999 9), 8.88—155.40(r = 0.999 9), 77.66—1 359.05(r = 0.999 9), 41.4—724.5(r = 0.999 9), 6.70—117.25(r = 0.999 9), and 25.50—446.25 ng(r = 0.999 9). The average recoveries(n = 6) were 98.2%(RSD = 2.0%), 99.6%(RSD = 2.8%), 100.2%(RSD = 1.3%), 99.0%(RSD = 2.2%), 100.8%(RSD = 2.6%), 98.7%(RSD = 2.5%), and 97.7%(RSD = 2.2%), respectively. Conclusion This method is simple and rapid, and can be used for the quality control of Cuyanhusuo Granule with satisfactory separation and repeatability.
引文
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[2]贺凯,高建莉,赵光树.延胡索化学成分、药理作用及质量控制研究进展[J].中草药,2007,38(12):1909-1912.
[3]蓝明雄.醋延胡索配方颗粒质量标准的研究[J].中国中医药咨询,2011,20(3):66-67.
[4]魏惠珍,谢菲,饶毅,等.HPLC法测定元胡止痛胶囊中延胡索乙素及其不确定度评定[J].中草药,2012,43(2):299-302.
[5]刘梅,汤树良,张文惠.HPLC色谱指纹图谱鉴别夏天无和延胡索药材[J].中药材,2003,26(9):629-631.
[6]张捷,黄荣华.HPLC测定延胡索不同炮制品中延胡索乙素含量[J].西北药学杂志,2006,21(5):209-210.
[7]王杰,刘冰,周军,等.六味地黄配方颗粒与传统汤剂中6种有效成分的比较研究[J].中草药,2015,46(19):2887-2891.
[8]孙源源,施萍.借助中药配方颗粒推进中药国际化的对策研究[J].中草药,2013,44(8):929-934.
[9]中国药典[S].一部.2010.
[10]王正宽,刘圆,周茆,等.中试规模下Box-Behnken法优化延胡索微波提取工艺[J].中草药,2015,46(16):2394-2399.