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目的:建立反相高效液相色谱-柱前衍生化法测定金糖宁胶囊中1-脱氧野尻霉素(1-DNJ)的含量。方法:样品经处理过的D001-CC型阳离子交换树脂上用氨水洗脱收集后,用2 g·L-1的芴甲氧羰酰氯(FMOC-C1)柱前衍生化,再采用高效液相色谱-二极管阵列检测器测定。ODS-C18色谱柱(4.0 mm×250 mm,5μm),流动相乙睛-0.2%磷酸溶液梯度洗脱,流速1.0 m L·min-1,检测波长263 nm,柱温25℃。结果:1-脱氧野尻霉素在0.84~8.4μg线性关系良好(r=1.000 0),精密度RSD0.3%,重复性RSD 0.6%,衍生化后的样品溶液在24 h内稳定,平均回收率109.6%,RSD 0.4%。结论:该方法稳定可靠,重复性好,精密度高,可用于金糖宁胶囊中1-脱氧野尻霉素的含量测定。
Objective: To establish a method for the determination of 1-deoxynojirimycin (1-DNJ) in jinhuning capsule by reversed-phase high performance liquid chromatography-precolumn derivatization. Methods: The samples were collected on D001-CC type cation exchange resin after being treated with ammonia water and pre-column derivatized with 2 g · L-1 fluorene methoxycarbonyl chloride (FMOC-C1) Chromatography - Diode Array Detector. ODS-C18 column (4.0 mm × 250 mm, 5 μm). The mobile phase was eluted with a gradient of acetonitrile-0.2% phosphoric acid. The flow rate was 1.0 mL min -1. The detection wavelength was 263 nm and the column temperature was 25 ℃. Results: The linearity of 1-deoxynojirimycin was good (r = 1.000 0) between 0.84 and 8.4 μg, the RSD of precision was 0.3% and the repeatability of RSD was 0.6%. The derivatized sample solution was stable within 24 h Rate of 109.6%, RSD 0.4%. Conclusion: The method is stable and reliable, good reproducibility, high precision, and can be used for the determination of 1-deoxynojirimycin in jinhuning capsule.