基于氨基柱的反相/正相液相色谱-电喷雾串联质谱法测定纺织品中的二硬脂基二甲基氯化铵  

Determination of distearyl dimethyl ammonium chloride in textiles by reversed-phase and normal-phase liquid chromatography-electrospray ionizationtandem mass spectrometry

作　　者：丁友超[1] 申晓萍[2] 吴晓琼[3] 吴丽娜[1] 曹锡忠[1] 

机构地区：[1]江苏出入境检验检疫局工业产品检测中心,江苏南京210001 [2]南通出入境检验检疫局综合技术中心,江苏南通226005 [3]南京化工职业技术学院应用化学系,江苏南京210048

出　　处：《色谱》2011年第6期507-512,共6页Chinese Journal of Chromatography

基　　金：国家"十一五"科技支撑计划重点项目(2006BAK10B03-3);质量检验公益性行业科研专项项目(200910013)

摘　　要：建立了纺织品中二硬酯基二甲基氯化铵(DSDMAC)的反相(RP)/正相(NP)液相色谱-电喷雾串联四极杆质谱(LC-ESI-MS/MS)的分析方法。选用甲醇为提取溶剂,确定了超声功率为420 W、提取温度为70℃的超声波辅助提取条件,实现了30 min快速提取样品中的DSDMAC。建立了基于氨基柱的反相和正相两套液相色谱分离系统,采用LC-MS/MS的选择反应监测(SRM)模式检测3个DSDMAC组分。结果显示:RPLC和NPLC对DSDMAC的检出限(S/N=3)分别为0.1 mg/kg和0.01 mg/kg。采用RPLC-MS/MS为定量方法,对8种不同的空白纤维纺织品的添加回收率为85.5%～103%(n=5);平行测试的相对标准偏差(RSD)为4.18%～12.8%(n=5)。5家外部实验室分别采用上述方法对2种参考样品中的DSDMAC进行检测,实验室间测定的RSD分别为7.3%和9.4%。该方法快速、准确、稳定,适用于纺织品中DSDMAC的检测。A method of reversed-phase（RP）/normal-phase（NP）-liquid chromatography-electrospray ionization-tandem mass spectrometry（LC-ESI-MS/MS） was developed for the determination of distearyl dimethyl ammonium chloride（DSDMAC） in textiles. The DSDMAC in textile was extracted by ultrasound-assisted extraction using methanol as extraction solvent under the conditions of 70 ℃ and 420 W within 30 min.The three quaternary ammonium compounds of DSDMAC were detected by LC-MS/MS in the selective reaction monitoring（SRM） mode.The limits of detection（LODs）（S/N=3） of DSDMAC detected by RPLC-MS/MS and NPLC-MS/MS based on an amino-column were 0.1 mg/kg and 0.01 mg/kg,respectively.The recoveries of DSDMAC spiked in the eight different types of blank fabrics ranged from 85.5% to 103% with the relative standard deviations（RSDs） of 4.18%-12.8%（n=5） by RPLC-MS/MS method.Five laboratories were invited to take part in the validation of the method,and the RSDs of inter-lab were 7.3%-9.4% on two reference samples.The method is fast,accurate and reproducible,and can meet the demands of the determination of DSDMAC in textiles.

关 键 词：反相/正相液相色谱 液相色谱-串联质谱 季铵盐化合物 二硬酯基二甲基氯化铵 纺织品 

分 类 号：O658[理学—分析化学]