超高效液相色谱法测定湿巾中7种防腐剂

建立超高效液相色谱法测定湿巾中7种防腐剂的检测方法。样品采用甲醇超声提取,色谱柱采用Waters ACQUITY UPLC BEH C_(18)柱(50 mm×2.1 mm,1.7μm),流动相为甲醇–乙酸水溶液(pH 3.3)梯度洗脱,初始流量为0.8 m L/min,用PDA检测器检测,检测波长分别为255,270,310 nm。以3倍空白噪音计,2-溴-2-硝基丙烷-1,3-二醇,苯酚,苯甲醇,苯氧乙醇,苯甲酸,山梨酸,脱氢乙酸的检出限分别为60.0,0.5,20.0,8.0,5.0,0.2,0.5 mg/kg;方法加标回收率为100.9%~109.3%;测定结果的相对标准偏差为0.2%~1.9%(n=6)。结果表明该方法处理简单,分离效果好,速度快,能快速准确测定湿巾中7种防腐剂。

Determination of 7 Preservatives in Wet Wipes by Ultra-Performance Liquid Chromatography

An UPLC (Ultra-Performance Liquid Chromatography) method was established for determination of the 7 preservatives in wet wipes. The sample was extracted by methanol using ultrasonic bath. The preservatives were separated on the Waters ACQUITY UPLC BEH C18 column(50 mm×2.1 mm,1.7 μm) by using methanol-acetic solution(pH 3.3) as the mobile phase at an initial flow rate of 0.8 mL/min, and detected by PDA detector on detecting wavelengths of 255, 270, 310 nm. The detection limits(S/N=3) of burnable, phenol, benzyl alcohol, phenoxyethanol, benzoic acid, sorbic acid, dehydroacetic were 60.0, 0.5, 20.0, 8.0, 5.0, 0.2, 0.5 mg/kg. The average recoveries for preservatives in wet wipes were 100.9%-109.3%. The relative standard deviations of determination results were 0.2%-1.9%(n=6). The sample pretreatment is simple, the extraction efficiency is high, and the separation is quick and effective. The method is suitable for determination of the 7 preservatives in wet wipes.