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目的建立反相高效液相色谱法测定不同月份高良姜中高良姜素含量的方法。方法采用液相色谱-质谱联用(LC-MS)进行峰识别和分离度判断,获得优化的色谱分离条件:Shim-pack VP-ODS柱(2.0 mm×250 mm,5μm),流动相A为0.1%HAc水溶液,流动相B为15%乙腈+40%甲醇+45%四氢呋喃,梯度洗脱程序为0～20 min、39%～61%B;20～30 min、61%～100%B;流速0.2 mL.min-1,柱温35℃,检测波长280 nm。结果高良姜素色谱峰的分离度大于1.5,高良姜素在0.020～0.64 g.L-1内呈良好线性,r=0.999 8;平均回收率为100.7%,RSD为2.82%(n=6)。结论本方法准确、精密度高、专属性好,可用于高良姜道地药材及其制剂的质量控制。
Objective To establish a method for the determination of galangin in galangal in different months by RP-HPLC. Methods The peak identification and resolution were determined by Liquid Chromatography-Mass Spectrometry (LC-MS). The optimized chromatographic separation conditions were: Shim-pack VP-ODS column (2.0 mm×250 mm, 5 μm). The mobile phase A was 0.1% HAc aqueous solution, mobile phase B is 15% acetonitrile + 40% methanol + 45% tetrahydrofuran, gradient elution program is 0 ~ 20 min, 39% ~ 61% B; 20 ~ 30 min, 61% ~ 100% B; The flow rate was 0.2 mL.min-1, the column temperature was 35°C, and the detection wavelength was 280 nm. Results The chromatographic peak separation of galangin was greater than 1.5, galangin was linear in 0.020-0.64 g.L-1, r=0.999 8, the average recovery was 100.7%, and the RSD was 2.82% (n=6). Conclusion The method is accurate, precise and specific. It can be used to control the quality of Gaoliangjiangdao herbs and its preparations.