Rodríguez-Gómez Rocío, Roldán-Pijuán Mercedes, Lucena Rafael, Cárdenas Soledad, Zafra-Gómez Alberto, Ballesteros Oscar, Navalón Alberto, Valcárcel Miguel
Research Group of Analytical Chemistry and Life Sciences, Department of Analytical Chemistry, Campus of Fuentenueva, University of Granada, E-18071 Granada, Spain.
Department of Analytical Chemistry, Institute of Fine Chemistry and Nanochemistry, Marie Curie Building, Campus of Rabanales, University of Córdoba, E-14071 Córdoba, Spain.
J Chromatogr A. 2014 Aug 8;1354:26-33. doi: 10.1016/j.chroma.2014.05.071. Epub 2014 Jun 2.
In this article, stir-membrane solid-liquid-liquid microextraction (SM-SLLME) is tailored for the analysis of solid matrices and it has been evaluated for the determination of parabens in l breast milk samples. A three-phase microextraction mode was used for the extraction of the target compounds taking advantage of their acid-base properties. The unit allows the simultaneous extraction of the target compounds from the solid sample to an organic media and the subsequent transference of the analytes to an aqueous acceptor phase. The method includes the identification and quantification of the analytes by ultra high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS). All the variables involved in the extraction procedure have been accurately studied and optimized. The analytes were detected and quantified using a triple quadrupole mass spectrometer (QqQ). The selection of two specific fragmentation transitions for each compound allowed simultaneous quantification and identification. The method has been analytically characterized on the basis of its linearity, sensitivity and precision. Limits of detection ranged from 0.1 to 0.2ngmL(-1) with precision better than 8%, (expressed as relative standard deviation). Relative recoveries were in the range from 91 to 106% which demonstrated the applicability of the stir-membrane solid-liquid-liquid microextraction for the proposed analytical problem. Moreover, the method has been satisfactorily applied for the determination of parabens in lyophilized breast milk samples from 10 randomly selected individuals.
在本文中，搅拌膜固液液微萃取（SM-SLLME）专为固体基质分析而设计，并已用于测定母乳样品中的对羟基苯甲酸酯。利用目标化合物的酸碱性质，采用三相微萃取模式萃取目标化合物。该装置可将目标化合物从固体样品中同时萃取到有机介质中，随后将分析物转移到水相接受相中。该方法包括通过超高效液相色谱-串联质谱（UHPLC-MS/MS）对分析物进行鉴定和定量。对萃取过程中涉及的所有变量进行了精确研究和优化。使用三重四极杆质谱仪（QqQ）对分析物进行检测和定量。为每种化合物选择两个特定的碎片跃迁，可实现同时定量和鉴定。该方法已根据其线性、灵敏度和精密度进行了分析表征。检测限范围为0.1至0.2 ng mL⁻¹，精密度优于8%（以相对标准偏差表示）。相对回收率在91%至106%之间，这表明搅拌膜固液液微萃取适用于所提出的分析问题。此外，该方法已成功应用于10名随机选择个体的冻干母乳样品中对羟基苯甲酸酯的测定。
