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目的建立液-质联用(LC-MS)法检测硫酸亚铁缓释片中邻苯二甲酸二辛酯(DOP)的含量。方法采用Waters BEHC18(50 mm×2.1 mm,1.7μm)色谱柱,流动相为95%甲醇-5%乙酸铵溶液梯度洗脱,流速为0.2 mL.min 1,柱温为35℃;质谱采用电喷雾离子源,多反应监测模式(正离子),两通道391→149,391→167。结果 DOP在0.091 3～0.913 0 ng内线性关系良好,回归方程为Y=268 462X+162 526(r=0.997 3);以加标样品计算,在低、中、高3个浓度水平下,DOP平均回收率为98.5%;定量限为0.05 ng,检测限为0.01 ng。结论本方法灵敏度高,结果准确可靠,适用于硫酸亚铁缓释片中DOP的含量检测。
Objective To establish a liquid-mass spectrometry (LC-MS) method for the determination of dioctyl phthalate (DOP) in ferrous sulfate sustained release tablets. Methods Waters BEHC18 (50 mm × 2.1 mm, 1.7 μm) was used as the mobile phase. The mobile phase consisted of gradient elution with 95% methanol-5% ammonium acetate solution at a flow rate of 0.2 mL · min 1 and a column temperature of 35 ℃. Spray ion source, multi-reaction monitoring mode (positive ion), two-channel 391 → 149,391 → 167. Results The linearity of DOP in the range of 0.091 3-0.913 0 ng was good and the regression equation was Y = 268 462X + 162 526 (r = 0.997 3). With the spiked samples, at the low, middle and high concentration levels, DOP The average recovery was 98.5%; the limit of quantification was 0.05 ng and the limit of detection was 0.01 ng. Conclusion The method has high sensitivity, accurate and reliable results and is suitable for the determination of DOP in ferrous sulfate sustained release tablets.