Department of Pharmaceutical Chemistry, Faculty of Pharmacy, King Abdulaziz University, P.O. Box 80260, Jeddah 21589, Saudi Arabia.
J Chromatogr B Analyt Technol Biomed Life Sci. 2013 Jul 1;930:98-103. doi: 10.1016/j.jchromb.2013.04.040. Epub 2013 May 10.
Described below is an optimized solid-phase extraction method (SPE) for the simultaneous determination of three hazardous plastic additives. Two high-performance liquid chromatographic-electrospray ionization-mass spectrometric (HPLC-ESI-MS) methods were developed and validated to estimate the melamine (MEL), bis(2-ethylhexyl) phthalate (DEHP), and bisphenol A (BPA) contents in drinking water, syringes, soft drinks, and dry milk powder. One extraction procedure optimally recovered all three substances from the different matrices. Two extraction columns were combined and included a silica gel LiChroprep RP-2 column (20:1, g/g, top column) and a Sep-Pak with a C18 column (500mg, bottom column). The analytical column was an Agilent Eclipse XDB-C8 column, 4.6mm×150mm, 5μm, maintained at 50±2°C. MEL and DEHP were monitored by positive triple quad mass spectrometry (TQ-MS) using an acidic mobile phase, while BPA was monitored by negative TQ-MS using a mobile phase containing a 0.05% ammonia solution. The general linear range of the three compounds ranged from 12 to 1000pg/μL in the injected solution (25μL). The average extraction recoveries were within the range of 83.0-102.5%. Relatively high concentrations of BPA and DEHP were found in the milk powder and sterile syringes.
下面描述了一种优化的固相萃取方法（SPE），用于同时测定三种危险的塑料添加剂。开发并验证了两种高效液相色谱-电喷雾电离质谱（HPLC-ESI-MS）方法，以估计饮用水、注射器、软饮料和奶粉中三聚氰胺（MEL）、邻苯二甲酸二（2-乙基己基）酯（DEHP）和双酚 A（BPA）的含量。一种提取程序从不同基质中最佳地回收了所有三种物质。两个萃取柱结合在一起，包括一个硅胶 LiChroprep RP-2 柱（20:1，g/g，上柱）和一个带有 C18 柱的 Sep-Pak（500mg，下柱）。分析柱为 Agilent Eclipse XDB-C8 柱，4.6mm×150mm，5μm，保持在 50±2°C。MEL 和 DEHP 通过酸性流动相进行正三重四极杆质谱（TQ-MS）监测，而 BPA 通过含有 0.05%氨溶液的流动相进行负 TQ-MS 监测。三种化合物的通用线性范围在 25μL 进样溶液中为 12-1000pg/μL。平均提取回收率在 83.0-102.5%范围内。在奶粉和无菌注射器中发现了相对较高浓度的 BPA 和 DEHP。
