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目的鉴定维C银翘片中非法添加物D-(-)-异抗坏血酸的结构,对样品进行添加物筛查。方法采用CAPCELL PAKNH2色谱柱(4.6 mm×250 mm,5μm),流动相为乙腈-20 mmol·L-1乙酸铵(甲酸调pH至2.5)(60∶40),检测波长为246 nm,流速为1 mL·min-1;离子源为ESI源,雾化气压力为220 kPa,干燥气流速为12 L·min-1,干燥气温度350℃,毛细管电压3.5kV,正离子检测。用液相色谱分离并制备维C银翘片中添加物,进行13 C-NMR结构确证。结果通过对检出的添加物[M+H]+多级质谱裂解规律解析及与D-(-)-异抗坏血酸对照品比较,鉴定添加物为D-(-)-异抗坏血酸;通过添加物13C-NMR化学位移分析,进一步确认其结构。在366批维C银翘片样品中,有64批样品检出非法添加物D-(-)-异抗坏血酸。结论液质联用方法准确,灵敏度高,可满足定性检测的要求。
Objective To identify the structure of D - (-) - isoascorbic acid, an illegal additive in vitamin C Yinqiao tablets, and to screen the samples for additives. Methods CAPCELL PAKNH2 column (4.6 mm × 250 mm, 5 μm) was used. The mobile phase consisted of acetonitrile-20 mmol·L-1 ammonium acetate (pH 6.0 to formic acid) (60:40). The detection wavelength was 246 nm and the flow rate was 1 mL · min-1. The ion source was the ESI source, the pressure of the atomization gas was 220 kPa, the flow rate of the drying gas was 12 L · min-1, the temperature of the drying gas was 350 ℃ and the capillary voltage was 3.5kV. The liquid chromatography was used to prepare and prepare the compound C Victoria Alice. The 13 C-NMR structure was confirmed. Results The analyte was identified as D - (-) - isoascorbic acid by analyzing the detected rule of [M + H] + multiple mass spectrometry and comparison with D - (-) - isoascorbic acid reference substance. 13C-NMR chemical shift analysis, to further confirm its structure. Of the 366 batches of C Yinqiao tablets, 64 batches of samples were found to be illegal additives D - (-) - erythorbic acid. Conclusion The method of LC-MS is accurate and sensitive, which can meet the requirements of qualitative detection.