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作 者:李全忠[1] 周明辉[1] 岳大磊[1] 郑建国[1] 刘莹峰[1] 翟翠萍[1]
出 处:《分析测试学报》2011年第12期1444-1447,共4页Journal of Instrumental Analysis
基 金:国家质检总局科研项目(2010IK039)
摘 要:建立了超声辅助萃取/液相色谱-串联质谱(LC-MS/MS)测定染整助剂中二硬脂基二甲基氯化铵(DSDMAC)的方法。将样品以甲醇为萃取溶剂进行超声萃取,萃取液经过滤后采用LC-MS/MS测定。采用电喷雾离子源,定性离子对为m/z 550.5/298.3、522.5/298.3、522.5/270.3、494.5/270.3;定量离子对为m/z 550.5/298.3、522.5/298.3、494.5/270.3。方法线性范围为0.02~1.0 mg/L,相关系数为0.998 5,方法的定量下限为20 mg/kg,在100~500 mg/kg范围的加标回收率为86%~96%,相对标准偏差为3.2%~5.4%。结果表明,该方法快速、准确、灵敏度高,能满足相关测定要求。An analytical method was established for the determination of distearyl dimethyl ammonium chloride(DSDMAC) in dyeing and finishing textile agents by ultrasound-assisted extraction combined with liquid chromatography - tandem mass spectrometry ( LC - MS/MS). The sample was extracted with methanol by ultrasound-assisted extraction. The extract was filtered and then detected by LC - MS/MS with electro-spray ionization source. The confirmation ion pairs were m/z 550. 5/298.3, 522.5/298.3, 522.5/270. 3, 494.5/270. 3, and the quantification ion pairs were m/z 550.5/ 298.3, 522.5/298.3, 494.5/270.3. The calibration curve was linear for DSDMAC in the range of 0.02 - 1.0 mg/L with correlation coefficient of 0. 998 5. The limit of quantitation was 20 mg/kg. The recoveries of DSDMAC at the spiked range of 100 - 500 mg/kg were between 86% and 96% , with relative standard deviations (RSDs) of 3.2% - 5.4%. The experimental results indicated that the method was rapid, sensitive and accurate, and could meet the correlative requirements for determination of DSDMAC in dyeing and finishing textile agents.
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