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目的建立HPLC-ELSD测定炉贝母不同提取物中贝母辛和贝母素乙含量的方法,研究采用不同提取方法时贝母辛和贝母素乙两生物碱含量的差异。方法采用HPLC-ELSD法进行分析;色谱柱:Comatex C18(5μm,250 mm×4.6mm);流动相:初始比例为乙腈∶0.02%三乙胺水溶液(38∶62),梯度洗脱;流速:1.0 ml·min-1;柱温:35℃;SofTA Model 300S ELSD参数:漂移管温度90℃,雾化室温度35℃,载气压力46.2 psi。结果贝母辛的进样量在2.750~9.625μg范围内,其进样浓度的对数(X=lgC)与峰面积积分值的对数(Y=lgA)具有良好的线性关系(Y=2.218 98+1.401 53X,r=0.999 8);贝母素乙的进样量在1.5~9.0μg范围内,其进样浓度的对数(X=lgC)与峰面积积分值的对数(Y=lgA)具有良好的线性关系(Y=2.516 79+1.132 66X,r=0.999 7)。结论该方法操作简便,可靠稳定,结果准确;回流提取法中贝母辛和贝母素乙含量均高于超声提取法和渗漉法,为探索炉贝母中异甾体生物碱类有效成分的提取提供了重要参考依据。
OBJECTIVE To establish a HPLC-ELSD method for the determination of Fritillaria and Fritillaria B in different extracts of Fritillaria cirrhosa, and to study the differences in the contents of Fritillaria and Fritillariae B alkaloids when using different extraction methods. The mobile phase consisted of acetonitrile: 0.02% triethylamine in water (38:62), gradient elution; flow rate: 1.0 ml · min-1; column temperature: 35 ℃; SofTA Model 300S ELSD parameters: drift tube temperature 90 ℃, atomization chamber temperature 35 ℃, carrier gas pressure 46.2 psi. Results The injection volume of Fritillaria in the range of 2.750 ~ 9.625μg, the logarithm of the injection concentration (X = lgC) and the peak area integral logarithm (Y = lgA) has a good linear relationship (Y = 2.218 98 + 1.401 53X, r = 0.999 8). The logarithm of logarithm of sample concentration (X = lgC) and the logarithm of peak area integral value (Y = lgA) had a good linear relationship (Y = 2.51679 + 1.132 66X, r = 0.999 7). Conclusion The method is simple, reliable and stable, and the results are accurate. The contents of Fritillaria and Peiminine B in reflux extraction method are higher than that of ultrasonic extraction and percolation method. In order to explore the effective components of the steroid alkaloids in Fritillaria cirrhosa, The extraction provides an important reference.