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    利用核-壳亚3微米填料色谱技术快速测定镇痛类健康产品中25种非法添加药物

    Rapid Determination of 25 Adulterated Drugs in Analgesic Health Products Based on Chromatography Technique with Fused-Core Sub-3 μm Filler

    • 摘要: 采用核-壳亚3微米填料色谱柱建立了快速测定镇痛类健康产品中25种非法添加解热镇痛类药物及糖皮质激素类药物的高效液相色谱法。样品经甲醇超声提取,用Phenomenex Kinetex XB-C18色谱柱(100 mm×4.6 mm,2.6 μm)分离,流动相为乙腈-甲醇(2+1)溶液和0.2 mol%#183;L-1乙酸铵溶液(pH 4.2),梯度洗脱。采用二极管阵列检测器,外标法定量。25种药物的线性范围为1.0~100 mg·L-1,检出限(3S/N)为0.02~0.10 g·kg-1。加标回收率为90.6%~110%,测定值的相对标准偏差(n=6)为0.42%~2.5%。方法用于分析66批镇痛类健康产品,发现24批阳性样品,检出8种药物成分。

       

      Abstract: High performance liquid chromatography (HPLC) method based on a fused-core sub-3 μm filler column was developed for the rapid determination of 25 drugs in analgesic health products. The samples were extracted ultrasonically with methanol, and the extract was separated on a Phenomenex Kinetex XB-C18 chromatographic column (100 mm×4.6 mm, 2.6 μm) with acetonitrile/methanol (2+1) and 0.2 mol·L-1 ammonium acetate solution (pH 4.2) as mobile phases for gradient elution. Diode array detector was used. Quantification analysis was performed by the external standard method. The same linearity range of 25 drugs was 1.0-100 mg·L-1, with detection limits (3S/N) ranged from 0.02 g·kg-1 to 0.10 g·kg-1. Recovery rates obtained by standard addition method ranged from 90.6% to 110% with RSDs (n=6) of 0.42%-2.5%. The method was applied for analysis of 66 analgesic health products, and 24 positive samples were found and 8 drugs were detected.

       

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