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目的:建立内消片中斑蝥素的含量测定方法。方法:采用DB-1型毛细管气相色谱柱(30 mm×0.32 mm,0.25μm)和FID检测器;以氮气为载气,流速为2 m L/min,进样口温度为225℃,检测器温度为250℃,分流比为10∶1;样品经粉碎后用三氯甲烷溶剂浸渍过夜,采用索氏提取法提取;测定内消片中斑蝥素的含量。结果:斑蝥素线性浓度范围在0.127~260.000μg/m L(r=0.999 9)内,高、中、低3种浓度的加样回收率高于94.66%(RSD为4.24%,n=5),重复性RSD为2.86%(n=5);3种浓度的精密度RSD低于1.51%(n=5);测得3批内消片中斑蝥素的平均含量为0.083 mg/g。结论:本方法简单、准确、可靠,可用于内消片中斑蝥素的含量测定。
Objective: To establish a method for the determination of cantharidin in Cixi tablet. Methods: DB-1 capillary column (30 mm × 0.32 mm, 0.25 μm) and FID detector were used. The flow rate of nitrogen was 2 mL / min and the inlet temperature was 225 ℃. The detector The temperature was 250 ℃, the split ratio was 10: 1; the sample was crushed and then impregnated with chloroform solvent overnight, extracted by Soxhlet extraction; Results: The linear range of cantharidin was 0.127 ~ 260.000μg / m L (r = 0.999 9). The recoveries of high, middle and low concentrations were higher than 94.66% (RSD 4.24%, n = 5) , RSD of repeatability was 2.86% (n = 5). The RSDs of the three concentrations were less than 1.51% (n = 5). The average content of cantharidin in the three batches of endocyts was 0.083 mg / g. Conclusion: The method is simple, accurate and reliable and can be used to determine the content of cantharidin in endocardial tablets.