摘要
目的:建立测定蛇胆汁中牛磺胆酸钠含量的高效液相色谱-电雾式检测器(HPLC-CAD)法,同时对紫外检测器、蒸发光检测器和电雾式检测器3种不同检测器的灵敏度进行比较。方法:采用ZORBAX SB C_(18)色谱柱(4.6 mm×250 mm,5μm),流动相为乙腈-0.1%三氟乙酸水(30∶70),等度洗脱,流速为1.0 mL·min^(-1),柱温35℃,CAD雾化温度35℃,气压4.206×10~5 Pa。结果:蛇胆汁进样量在0.174 2~3.484 0μg范围内与峰面积线性关系良好(r=0.999 5),平均回收率为99.0%,RSD为0.76%(n=6),阴性对照无干扰。本实验测得牛磺胆酸钠含量范围眼镜蛇科为5.69~28.85 mg·g^(-1);游蛇科为23.37~29.65 mg·g^(-1);蝰科为6.54~24.00 mg·g^(-1)。结论:该方法经方法学验证,可作为蛇胆汁质量控制的方法。
Objective： To establish an HPLC-CAD method for determination of Sodium taurocholate in snake bile, and to compare the sensitivity of three different detectors of ultraviolet detector （ UV ）, evaporative light scattering detector（ ELSD ）and charged aerosol detector （CAD）. Methods： ZORBAX SB CIs chromatographic column （ 4.6 mm ×250 mm,5μm ） was used; mobile phase was acetonitrile ： 0.1% trifluoroacetic acid （ 30：70 ） at a flow rate of 1.0 mL. min^-1 ; the column temperature was 35℃ ; the detector was CAD （ the spray temperature was 35 ℃ ）, at gas pressure of 4.206 × 10^5 Pa. Results： The snake bile showed good linear rang with 0.174 2-3.484 μg （ r=0.999 5 ） ; the average recovery was 99.0% ; RSD was 0.76% （ n=6 ） ; and the negative control had no interference. The measured contents of sodium taurocholate were 5.69-28.85 mg·g^-1 for Elapidaerang, 23.37- 29.65 mg·g^-1 for Colubridaeas, and 6.54-24.00 mg·g^-1 for Viperidaeas. Conclusion： The method can be used for the quality control of snake bile.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2017年第7期1223-1227,共5页
Chinese Journal of Pharmaceutical Analysis
基金
2015年安徽省科技攻关计划项目资助(1501041174)
