HPLC-ELSD法同时测定浙贝母饮片硫熏前后3种有效成分的含量

目的: 建立一种同时测定浙贝母饮片中贝母素甲、贝母素乙和贝母辛含量的方法,并比较硫熏对其含量的影响。方法: 采用高效液相色谱-蒸发光散射检测法(HPLC-ELSD),使用Agilent Eclipse C₁₈色谱柱(250 mm×4.6 mm,5 μm),以0.01%的二乙胺水溶液(A)-乙腈(B)为流动相,梯度洗脱(0~10 min,30%B;10~15 min,30%B→38%B;15~25 min,38%B→60%B;25~35 min,60%B;35~50 min,60%B→70%B;50~70 min,70%B→90%B),流速1 mL·min^-1,柱温30 ℃,漂移管温度为57 ℃,载气流速2.0 L·min^-1; 结果: 3种成分的峰面积对数值与浓度对数值的线性关系良好(r≥0.999 6),平均加样回收率(n=6)分别为99.05%、100.4%和100.8%;4个不同产地的浙贝母鲜切样品中贝母素甲、贝母素乙、贝母辛的含量分别为0.082%~0.133%、0.052%~0.063%、0.043%,硫熏样品中贝母素甲、贝母素乙、贝母辛的含量分别为0.062%~0.123%、0.033%~0.043%、0.012%;经硫熏后,浙贝母饮片中3种成分的含量均明显降低,贝母素甲降低了7.95%~32.66%,贝母素乙降低了20.38%~37.37%,贝母辛降低了71.44%~72.57%。结论: 所建立的方法简单、准确,重现性好,可作为评价和控制浙贝母饮片的质量的依据;硫熏会降低贝母饮片的贝母素甲、贝母素乙、贝母辛含量。

Objective: To establish a method for simultaneous determination of peimine,peiminine and peimisine in Zhejiang Fritillary slices,and compare the contents of the three constituents in Zhejiang Fritillary slices before and after sulfur-fumigating process. Methods: The samples were determined by HPLC-ELSD with an Agilent Eclipse C₁₈ column(250 mm×4.6 mm,5 μm) using 0.01% diethylamine water solution(A)-acetonitrile(B) as the mobile phase by gradient elution(0-10 min,30%B;10-15 min,30%B→38%B;15-25 min,38%B→60%B;25-35 min,60%B;35-50 min,60%B→70%B;50-70 min,70%B→90%B) at the flow rate of 1 mL·min^-1.The carrier gas flow rate was 2.0 L·min^-1,and the temperatures of column and drift tube were maintained at 30 ℃ and 57 ℃,respectively. Results: All the constituents showed good linearity(r≥0.999 6) in the range of the tested concentration.The average recoveries(n=6) of the method were 99.05%,100.4% and 100.8%,respectively.The contents of the three constituents in fresh-cut Zhejiang Fritillary slices from four different origins were 0.082%-0.133%,0.052%-0.063%,0.043%,respectively;and those in sulphur-fumigated slices were 0.062%-0.123%,0.033%-0.043%,0.012%,respectively.After sulfur-fumigating process,the contents of the three constituents in Zhejiang Fritillary slices decreased obviously,as peimine decreased by 7.95%-32.66%,peiminine by 20.38%-37.37%,and peimisine by 71.44%-72.57%,respectively. Conclusion: The validated method has the advantages of simplicity,good precision and reliability,allowing the comprehensive quality control of Zhejiang Fritillary slices.Sulfur fumigation reduces the contents of peimine,peiminine and peimisine in Zhejiang Fritillary slices.