HPLC法同时测定云连药材中6种生物碱的含量

Simultaneous Determination of 6 Alkaloids in Coptis teeta by HPLC

目的:建立同时测定云连药材中6种生物碱含量的方法。方法:色谱柱为Xtimate～(TM)C_(18),流动相为30 mmol/L碳酸氢铵溶液(含0.1%三乙胺和0.7%氨水)-乙腈(梯度洗脱),流速为1.0 mL/min,检测波长为270 nm,柱温为30℃,进样量为10μL。结果:药根碱、非洲防己碱、表小檗碱、黄连碱、盐酸巴马汀、盐酸小檗碱的检测质量浓度线性范围分别为0.85～16.96 mg/L(r=0.999 9)、1.25～24.96 mg/L(r=0.999 8)、2.05～40.96 mg/L(r=0.999 9)、3.65～72.96 mg/L(r=0.999 9)、2.88～57.60 mg/L(r=0.999 9)、13.25～264.96 mg/L(r=0.999 9);精密度、稳定性、重复性试验的RSD<3.0%;加样回收率分别为97.14%～102.14%(RSD=1.93%,n=6)、97.00%～102.00%(RSD=2.06%,n=6)、98.18%～101.82%(RSD=1.79%,n=6)、96.15%～101.28%(RSD=2.06%,n=6)、96.88%～101.88%(RSD=1.87%,n=6)、99.31%～103.76%(RSD=1.89%,n=6)。结论:该方法操作简便,精密度、稳定性、重复性好,可用于云连药材中6种生物碱含量的同时测定。

OBJECTIVE： To develop a method for simultaneous determination of 6 alkaloids in Coptis teeta. METHODS： The determination was performed on XtimateTM C18 with mobile phase consisted of 30 mmol/L ammonium bicarbonate [containing 0.1% triethylamine and 0.7% ammonia-acetonitrile （gradient elution）] at the flow rate of 1.0 mL/min. The detection wavelength was set at 270 nm, the column temperature was 30 ℃ ,and the sample size was 10μL. RESULTS： The linear ranges of jateorrhizine, co- lumbamine, epiberberine, coptisine, palmatine hydrochloride and berberine hydrochloride were 0.85-16.96 mg/L （r=0.999 9）, 1.25-24.96 mg/L（r=0.999 8）, 2.05-40.96 mg/L（r=0.999 9）, 3.65-72.96 mg/L（r=0.999 9）, 2.88-57.60 mg/L（r=0.999 9） and 13.25-264.96 mg/L（r=0.999 9）, respectively. RSDs of precision, stability and reproducibility tests were all lower than 3.0%. Re- coveries were 97.14%-102.14% （RSD= 1.93%, n=6）, 97.00%-102.00% （RSD=2.06%, n=6）, 98.18%-101.82% （RSD=1.79%, n=6）, 96.15%-101.28% （RSD=2.06% ,n=6）, 96.88%-101.88% （RSD= 1.87% ,n=6）, 99.31%-103.76% （RSD= 1.89% ,n= 6）, respectively. CONCLUSIONS： The method is simple, accurate, stability and reproducible, and can be used for simultaneous determination of 6 alkaloids in Coptis teeta.