Saraji Mohammad, Mirmahdieh Shiva
Department of Chemistry, Isfahan University of Technology, Isfahan, Iran.
J Sep Sci. 2009 Apr;32(7):988-95. doi: 10.1002/jssc.200800635.
A single-drop microextraction (SDME) method followed by in-syringe derivatization and GC-MS determination has been developed for analysis of five parabens, including methyl, ethyl, isopropyl, n-propyl and n-butyl paraben in water samples and cosmetic products. N,O-Bis(trimethylsilyl)acetamide (BSA) was used as derivatization reagent. Derivatization reaction was performed inside the syringe barrel using 0.4 microL of BSA. Parameters that affect the derivatization yield such as temperature and time of the reaction were studied. In addition, experimental SDME parameters such as selection of organic solvent, addition of salt, extraction time and extraction temperature were investigated and optimized. The RSD of the method for aqueous samples varied from 8.1 to 13%. The LODs ranged from 0.001 (n-butyl paraben) to 0.015 (methyl paraben) microg/L, and the enrichment factors were between 23 and 150.
已开发出一种单滴微萃取(SDME)方法,随后进行注射器内衍生化和气相色谱 - 质谱(GC-MS)测定,用于分析水样和化妆品中的五种对羟基苯甲酸酯,包括对羟基苯甲酸甲酯、乙酯、异丙酯、正丙酯和正丁酯。N,O-双(三甲基硅基)乙酰胺(BSA)用作衍生化试剂。使用0.4微升的BSA在注射器筒内进行衍生化反应。研究了影响衍生化产率的参数,如反应温度和时间。此外,还对实验性SDME参数,如有机溶剂的选择、盐的添加、萃取时间和萃取温度进行了研究和优化。该方法对水样的相对标准偏差(RSD)在8.1%至13%之间。检测限(LOD)范围为0.001(对羟基苯甲酸正丁酯)至0.015(对羟基苯甲酸甲酯)微克/升,富集因子在23至150之间。