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利用超声萃取高效液相色谱分离紫外检测,建立了化妆品中14种磺胺类物质的分离测定方法。优化了影响萃取效率的因素(包括有机溶剂种类、萃取时间、萃取温度和超声频率)。实验结果表明,最佳萃取条件为:萃取剂为甲醇,萃取时间为25 min,超声频率为45 kHz,萃取温度为25℃。分离条件为:依利特Hypersil ODS柱分离,流动相为乙腈和体积分数0.5%乙酸水溶液(梯度洗脱),流速1.0 mL/min,柱温30℃,检测波长为272 nm。方法拥有良好的线性(r≥0.9998)、检出限(≤0.12 mg/L)、回收率(83.9%~113%)和重现性(RSD≤0.83%,n=8),可用于复杂基质样品中磺胺类化合物的测定。
The separation and determination of 14 sulfonamides in cosmetics were established by ultrasonication and UV detection. Factors affecting extraction efficiency are optimized (including organic solvent type, extraction time, extraction temperature and ultrasonic frequency). The experimental results show that the optimum extraction conditions are as follows: the extractant is methanol, the extraction time is 25 min, the ultrasonic frequency is 45 kHz and the extraction temperature is 25 ℃. The separation conditions were: elite Hypersil ODS column, the mobile phase was acetonitrile and the volume fraction of 0.5% acetic acid in water (gradient elution), the flow rate was 1.0 mL / min, the column temperature was 30 ℃ and the detection wavelength was 272 nm. The method has good linearity (r≥0.9998), detection limit (≤0.12 mg / L), recovery (83.9% ~ 113%) and reproducibility (RSD≤0.83%, n = 8) Determination of sulfonamides in samples.