高效液相色谱法测定牙膏中的氨甲环酸

摘要

建立了丹磺酰氯柱前衍生/高效液相色谱测定牙膏中氨甲环酸(TA)的方法.牙膏经甲醇提取、氮吹至干,再用丹磺酰氯进行衍生.衍生物通过X-Bridge C18色谱柱(250 mm×4.6 mm×5μm)分离,以乙腈和0.1％甲酸水溶液为流动相梯度洗脱,在紫外波长250 nm条件下进行定量测定.系统考察了缓冲溶液pH值、衍生温度和衍生时间对氨甲环酸衍生效率的影响.结果表明,在优化实验条件下,氨甲环酸衍生物与基体杂质达到有效分离,在1～425 mg/L范围内线性关系良好,相关系数为0.999 5;在20,200,1 600 mg/kg 3个加标浓度下的回收率为98.7％ ～ 102％,相对标准偏差为0.85％ ～2.5％,方法检出限为2.0 mg/kg.该方法准确、可靠、灵敏度高,适用于各类牙膏中氨甲环酸的测定.%A high performance liquid chromatographic (HPLC) method was developed for the determination of tranexamic acid (TA) in toothpaste.Sample was extracted with methanol,and the extract was evaporated to dryness under nitrogen before it was derived with dansyl chloride.Chromatographic separation was performed on an X-Bridge C1s(250 mm ×4.6 mm ×5 μm) column using 0.1％ formic acid-acetonitrile mixture aqueous solution as mobile phase.The ultraviolet detection wavelength was set at 250 nm.Effects of pH value of buffer solution,reaction temperature and time were investigated.Under the optimized experimental conditions,the TA derivative was successfully separated from the other impurities,and showed a good linearity in the range of 1-425 mg/L with a correlation coefficient(r) of 0.999 5.At three spiked concentrations of 20,200,1 600 mg/kg,the recoveries ranged from 98.7％ to 102％ with relative standard deviations(RSDs) of 0.85％-2.5％.The limit of detection for this method was 2.0 mg/kg.With the advantages of accuracy,reliability and high sensitivity,this method was suitable for the determination of tranexamic acid in different kinds of toothpaste.