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目的:建立藏药珍珠丸系列品种(二十五味珍珠丸、七十味珍珠丸)中名贵药味西红花和牛黄所含6种组分(西红花苷-Ⅰ,西红花苷-Ⅱ、牛磺胆酸钠、胆酸、猪去氧胆酸、去氧胆酸)含量的HPLC-TUV-ELSD同时测定方法 ,并对不同企业的样品进行测定和分析。方法:采用Zorbax SB-C18色谱柱(4.6 mm×250 mm,5μm),流动相A为乙腈,B为1%甲酸,梯度洗脱程序为0~60 min,18%A~40%A,流速为1.0mL·min-1,柱温30℃,TUV检测波长为440 nm,ELSD漂移管温度80℃,雾化气压力为30 psi。结果:在选定的条件下,西红花苷-Ⅰ,西红花苷-Ⅱ、牛磺胆酸钠、胆酸、猪去氧胆酸、去氧胆酸6种组分分离良好,线性范围合理(r>0.993 2),加样回收率范围为97.5%~102.1%(n=6),LOD分别为0.000 1,0.000 2,0.005,0.002,0.003,0.002 g·L-1。结论:所建立的方法简便、快速、准确,能用于同时检测珍珠丸系列样品中6种组分的含量,为方中名贵药味的质量控制提供技术参考,并对市售样品进行质量分析。
OBJECTIVE: To establish the six components (crocin-Ⅰ, crocin-cortex safrole) contained in the precious medicinal herb saffron and bezoar in the Tibetan pearl pill series (Twenty-five pearl pill, seventy flavor pearl pill) Ⅱ, sodium taurocholate, cholic acid, hyodeoxycholic acid and deoxycholic acid) were determined by HPLC-TUV-ELSD. The samples of different enterprises were determined and analyzed. Methods: Zorbax SB-C18 column (4.6 mm × 250 mm, 5 μm) was used. The mobile phase A was acetonitrile and B was 1% formic acid. The gradient elution program was 0-60 min, 18% A -40% 1.0 mL · min-1. The column temperature was 30 ℃. The TUV detection wavelength was 440 nm, the ELSD drift tube temperature was 80 ℃ and the atomization gas pressure was 30 psi. Results: The six components of crocin-Ⅰ, crocin-Ⅱ, sodium taurocholate, cholic acid, hyodeoxycholic acid and deoxycholic acid were separated well under the selected conditions. The linear range The recoveries ranged from 97.5% to 102.1% (n = 6), and the LODs were 0.000, 1.000, 2.0.005, 0.002, 0.003 and 0.002 g · L-1, respectively. Conclusion: The established method is simple, rapid and accurate and can be used for the simultaneous determination of six components in the sample of pearl pills. It provides a technical reference for the quality control of the valuable medicines in the prescription and carries on the quality analysis on commercially available samples.