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目的:建立SPE-HPLC法测定金鸡胶囊中盐酸药根碱、盐酸巴马汀和盐酸小檗碱三种生物碱的含量。方法:选用WCX弱阳离子交换固相萃取小柱净化,采用Hvydro-RP 80A C_(18)柱(250 mm×4.6 mm,5μm),乙睛-0.05 mol·L~(-1)磷酸二氢钠溶液(磷酸调pH2.8)(27:73)为流动相,柱温35℃,流速1.0 ml·min~(-1),检测波长为265 nm。结果:盐酸药根碱、盐酸巴马汀、盐酸小檗碱分别在4.94～49.44 ng(r=1.000 0)、4.36～43.60 ng(r=0.999 9)和3.99～39.94 ng(r=0.999 9)范围内线性关系良好,回收率分别为99.32%(RSD=2.2%)、101.78%(RSD=1.7%)和103.19%(RSD=1.5%)(n=9)。结论:该方法操作简便,准确性、重复性好,可用于金鸡胶囊中盐酸小檗碱、盐酸巴马汀和盐酸药根碱的含量测定。
OBJECTIVE: To establish a SPE-HPLC method for the determination of three alkaloids in jinji capsule, such as jatrorrhizine hydrochloride, palmatine hydrochloride and berberine hydrochloride. Methods: WCX weak cation exchange solid phase extraction cartridges were used for purification. Hvydro-RP 80A C 18 column (250 mm × 4.6 mm, 5 μm), acetonitrile-0.05 mol·L -1 sodium dihydrogen phosphate The solution was adjusted to pH 2.8 with phosphoric acid (27:73) and the column temperature was 35 ℃. The flow rate was 1.0 ml · min -1 and the detection wavelength was 265 nm. Results: The parameters of jatrorrhizine hydrochloride, palmatine hydrochloride and berberine hydrochloride were 4.94-49.44 ng (r = 1.000 0), 4.36-43.60 ng (r = 0.999 9) and 3.99-39.94 ng (r = 0.999 9) The linearity was good with recoveries of 99.32% (RSD = 2.2%), 101.78% (RSD = 1.7%) and 103.19% (RSD = 1.5%), respectively (n = 9). Conclusion: The method is simple, accurate and reproducible. It can be used for the determination of berberine hydrochloride, palmatine hydrochloride and jatrorrhizine hydrochloride in Jinji Capsules.