【摘要】 建立了液相色谱-四极杆飞行时间质谱同时测定椰油酰胺丙基甜菜碱表面活性剂中一氯乙酸、二氯乙酸和羟基乙酸的方法。样品经水溶解后固相萃取小柱净化,经核壳型亚3μm填料色谱柱Agilent Poroshell 120 EC-C18(3.0 mm×100 mm×2.7μm)分离,以0.1%(V/V)甲酸和乙腈为流动相梯度洗脱,采用电喷雾离子源负离子全扫描模式采集后,提取精确离子定性定量。经方法验证3种化合物在一定质量浓度范围内线性良好,相关系数均大于0.997,3个添加水平的平均回收率在71.1%～92.2%之间,相对标准偏差(RSD)小于15%,方法检出限分别为:一氯乙酸0.25 mg/kg,二氯乙酸0.025 mg/kg,羟基乙酸10 mg/kg。更多还原

【Abstract】 A method based on ultra-high performance liquid chromatography with quadrupole time-of-flight mass spectrometry(UPLC-Q-TOF-MS) had been developed for the simultaneous determination of monochloroacetic acid, dichloroacetic acid and glycollic acid in cocamidopropyl betaine surfactant. The samples were dissolved by water, then purified by solid phase extraction and separated by a core-shell sub-3 μm column Agilent Poroshell120 EC-C18(3.0 mm×100 mm×2.7 μm) with a gradient elution of 0.1% formic acid and acetonitrile. Under electrospray ion source negative ion full scan mode, the extracted accurate ion was used to do qualitative and quantitative determination. The results show that the linearity of the three compounds is good in a certain concentration range, and the correlation coefficients are greater than 0.998. The average recovery of the three levels ranges from 71.1% to 92.2%, and the relative standard deviation(RSD) is less than 15%. The detection limits of the optimized method are 0.25 mg/kg for monochloroacetic acid, 0.025 mg/kg for dichloroacetic acid and10 mg/kg for glycollic acid.更多还原