表面解吸常压化学电离质谱法直接测定日化用品中1,4-二恶烷
MS/MS Direct Determination of 1,4-Dioxane in Daily Chemo-necessities with Surface Desorption Atmospheric Pressure Chemical Ionization
摘 要
在无需样品预处理的前提下,将表面解吸常压化学电离质谱法用于日化用品中1,4-二恶烷的直接快速检测。在串联质谱中,选择表面解吸常压化学电离离子源,以碰撞诱导解离反应正离子检测模式进行定性和定量检测。确定了1,4-二恶烷的碎片特征峰分别为m/z 72,45,61和32。1,4-二恶烷的线性范围为0.1~1 000 mg·L-1,检出限(3σ)为7.8×10-3mg·L-1。方法用于洗手液和洗发水的分析,回收率在84.7%~98.5%之间、测定值的相对标准偏差(n=6)在10%~18%之间。
1,4-二恶烷
日化用品
直接测定
Surface desorption atmospheric pressure chemical ionization-MS/MS
1,4-Dioxane
Daily chemo-necessities
Direct determination
Abstract
Surface desorption atmospheric pressure chemical ionization-tandem mass spectrometry (SDAPCI-MS/MS) was applied to the direct and rapid determination of 1,4-dioxane in daily chemo-necessities, without sample preparation and pretreatment. In the MS/MS analysis, SDAPCI was used as ion source, and positive electrospray ionization as well as collision induced dissociation reaction monitoring mode was taken for qualitative and quantitative analysis. The characteristic peaks of the fragments of 1,4-dioxane at m/z 72, 45, 61 and 32 respectively were confirmed. Linearity range of 1,4-dioxane was kept in the range of 0.1-1 000 mg·L-1, with value of detection limit (3σ) of 7.8×10-3mg·L-1. The proposed method was used in the analysis of samples of hand lotion and shampoo, giving values of recovery and RSD′s in ranges of 84.7%-98.5% and 10%-18% respectively.
中图分类号 O657.63
所属栏目 试验与研究
基金项目 国家自然科学基金(21165002);江西省自然科学基金(20114BAB203016);江西省教育厅科技基金(GJJ10504)资助
收稿日期 2011/10/27
修改稿日期
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备注杨水平(1963-),男,江西金溪人,副教授,学士,主要从事分析化学研究。
引用该论文: YANG Shui-ping,ZHANG Yan,WANG Jiang,JIA Bin,HU Bin,YIN Bang-da,ZHANG Hua,CHEN Huan-wen*. MS/MS Direct Determination of 1,4-Dioxane in Daily Chemo-necessities with Surface Desorption Atmospheric Pressure Chemical Ionization[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2012, 48(11): 1270～1273
杨水平,张燕,王姜,贾滨,胡斌,尹帮达,张华,陈焕文. 表面解吸常压化学电离质谱法直接测定日化用品中1,4-二恶烷[J]. 理化检验－化学分册, 2012, 48(11): 1270～1273
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【3】奚星林,钟崇泳,陈捷,等.顶空固相微萃取-气相色谱联用技术监测水相中的1,4-二恶烷［J］.中国卫生检验杂质, 2003,13(4):452-454.
【4】顾红.药物合成过程中有机溶剂残留量的检测［J］.天津化工, 2004,18(6):52-54.
【5】SCALIA S J. Reversed-phase high-performance liquid chromatographic method for the assay of 1,4-dioxane in sulphated polyoxyethylene alcohol surfactants［J］. Pharm Biomed Anal, 1990,8:867-870.
【6】黄业茹,施钧慧,唐莉.固相萃取工业废水中二恶烷的GC/MS分析［J］.质谱学报, 2001,22(1):69-74.
【7】TAKATS Z, WISEMAN J M, GOLOGAN B, et al. Mass spectrometry sampling under ambient conditions with desorption electrospray ionization［J］. Science, 2004,306(5695):471-473.
【8】胡燕,陈焕文,花榕,等.电喷雾解吸电离质谱法检测多种物质表面黑索今［J］.理化检验-化学分册,2009,45(5):504-507.
【9】陈焕文,胡斌,张燮.复杂样品质谱分析技术的原理及应用［J］.分析化学, 2010,38(8):1069-1088.
【10】杨水平,陈焕文,杨宇玲,等.鸡蛋中三聚氰胺的表面解吸常压化学电离串联质谱法成像［J］.分析化学, 2009,37(3):315-318.
【11】WU Zhong-chen, CHEN Huan-wen, WANG Wei-ling, et al. Differentiation of dried sea cucumber products from different geographical areas by surface desorption atmospheric pressure chemical ionization mass spectrometry［J］. J Agric Food Chem, 2009,57(20):9356-9364.
【12】WANG Jiang, YANG Shui-ping, YAN Fei-yan, et al. Rapid determination of dimethoate in nanoliter of juice using surface desorption atmospheric pressure chemical ionization mass spectrometry［J］. Chin J Anal Chem, 2010,38(4):453-457.
【13】YANG Shui-ping, DING Jian-hua, ZHENG Jian, et al. Detection of melamine in milk products by surface desorption atmospheric pressure chemical ionization mass spectrometry［J］. Anal Chem, 2009,81(7):2426-2436.
【14】CHEN Huan-wen, ZHENG Jian, ZHANG Xie, et al. Surface desorption atmospheric pressure chemical ionization mass spectrometry for direct ambient sample analysis without toxic chemical contamination［J］. Chinese J Anal Chem, 2007,42(8):1045-1056.
【15】陈焕文,赖劲虎,周瑜芬,等.表面解吸常压化学电离源的研制和应用［J］.分析化学, 2007,35(8):1233-1240.
【16】CHEN Huan-wen, LIANG Hua-zheng, DING Jian-hua, et al. Rapid differentiation of tea products by surface desorption atmospheric pressure chemical ionization mass spectrometry［J］. J Agric Food Chem, 2007,55(25):10093-10100.
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