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目的建立苦参碱微乳中苦参碱含量的气相色谱串联质谱(GC-MS)测定方法。方法 AgilentHP-5MS(30m,0.25mm×0.5μm)色谱柱,正二十三烷为内标,初始柱温为130℃,程序升温至280℃;EI离子源,正二十三烷和苦参碱的选择检测离子分别为m/z324.1和248.2。结果苦参碱含量在40～800μg/L范围内线性关系良好(r=0.9995),低(40μg/L)、中(160μg/L)、高(800μg/L)浓度的平均加样回收率分别为98.81%、100.20%和100.73%。结论 GC-MS法操作简便,结果准确,灵敏度高,重现性好,可用于苦参碱微乳制剂的质量控制。
Objective To establish a method for the determination of matrine in matrine microemulsion by gas chromatography-tandem mass spectrometry (GC-MS). Methods AgilentHP-5MS (30m, 0.25mm × 0.5μm) column was used with n-tricosane as the internal standard. The initial column temperature was 130 ℃ and the temperature was raised to 280 ℃. The EI ion source, n-tricosane and Sophora flavescens The base selected for detection of ions were m / z 324.1 and 248.2, respectively. Results The average recovery of matrine in the range of 40 ~ 800μg / L was good (r = 0.9995), and the average recovery was 40μg / L, 160μg / L and 800μg / L respectively 98.81%, 100.20% and 100.73% respectively. Conclusion GC-MS method is simple, accurate, sensitive and reproducible. It can be used for the quality control of matrine microemulsion.