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    柱前衍生-超高效液相色谱-电化学检测法测定牙膏中氨甲环酸

    Determination of Tranexamic Acid in Toothpaste by Pre-Column Derivatization Coupled with UPLC-ECD

    • 摘要: 约1 g牙膏样品用水50 mL超声萃取30 min后再离心10 min,然后取上清液加入等体积的衍生试剂溶液含有150 mg·L-1邻苯二甲醛(OPA)和1.3 g·L-1亚硫酸钠,在室温下反应5 min,完成对氨甲环酸的衍生化,衍生化后的样品溶液用超高效液相色谱-电化学检测器(UPLC-ECD)分析。采用Waters ACQUITY UPLC BEH C18色谱柱作为固定相,以体积比为2∶8的乙腈-30 mmol·L-1乙酸铵缓冲溶液(pH 3.6)为流动相进行等度洗脱。结果显示:氨甲环酸的质量浓度在0.495~19.800 mg·L-1内与其对应的色谱峰面积呈线性关系,检出限(3S/N)为0.18 μg·g-1。对牙膏样品进行了加标回收试验,回收率为98.6%,测定值的相对标准偏差(n=6)为2.4%。氨甲环酸衍生产物在12 h内保持稳定(衍生产物峰面积降低了不到5%)。方法用于6个牙膏样品的分析,在已知添加的牙膏样品中检出了氨甲环酸,其质量分数为0.23 mg·g-1

       

      Abstract: Tranexamic acid in the ca. 1 g of toothpaste sample was extracted with 50 mL of water by ultrasound for 30 min. After centrifuging for 10 min, the supernatant was reacted with the same volume of derivative reagent solution (containing 150 mg·L-1 OPA and 1.3 g·L-1 sulfite) at room temperature for 5 min. Sample solution after derivatization was analyzed by UPLC-ECD. Waters ACQUITY UPLC BEH C18 column was selected as the stationary phase, and the mixture of acetonitrile and 30 mmol·L-1 ammonium acetate buffer solution (pH 3.6) at a volume ratio of 2:8 was used as the mobile phase in the isocratic elution. The results showed that a good linear relationship between mass concentration of tranexamic acid and its respective peak area was found in the range of 0.495-19.800 mg·L-1, with detection limit of 0.18 μg·g-1. Recovery test was made by standard addition method in the toothpaste sample, and value of recovery obtained was 98.6%, with RSD (n=6) of determined values of 2.4%. The derivatization product was stable within 12 hours when its peak area reduced by less than 5%. The proposed method was used to analyze the 6 toothpaste samples, tranexamic acid with mass fraction of 0.23 mg·g-1 was found in one sample known to be added.

       

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