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超声辅助乳化微萃取-气相色谱串联质谱法测定葡萄酒中的 2,4,6-三氯苯甲醚

Ultrasound-assisted emulsification microextraction for determination of 2,4,6-trichloroanisole in wine samples by gas chromatography tandem mass spectrometry.

机构信息

Grupo de Investigacion y Desarrollo en Quimica Analitica (QUIANID) (LISAMEN, CCT CONICET-Mendoza), Mendoza, Argentina.

出版信息

J Agric Food Chem. 2010 Apr 28;58(8):4576-81. doi: 10.1021/jf904396g.

Abstract

A fast and effective microextraction technique is proposed for preconcentration of 2,4,6-trichloroanisole (2,4,6-TCA) from wine samples prior gas chromatography tandem mass spectrometric (GC-MS/MS) analysis. The proposed technique is based on ultrasonication (US) for favoring the emulsification phenomenon during the extraction stage. Several variables influencing the relative response of the target analyte were studied and optimized. Under optimal experimental conditions, 2,4,6-TCA was quantitatively extracted achieving enhancement factors (EF) > or = 400 and limits of detection (LODs) 0.6-0.7 ng L(-1) with relative standard deviations (RSDs) < or = 11.3%, when 10 ng L(-1) 2,4,6-TCA standard-wine sample blend was analyzed. The calibration graphs for white and red wine were linear within the range of 5-1000 ng L(-1), and estimation coefficients (r(2)) were > or = 0.9995. Validation of the methodology was carried out by standard addition method at two concentrations (10 and 50 ng L(-1)) achieving recoveries >80% indicating satisfactory robustness of the method. The methodology was successfully applied for determination of 2,4,6-TCA in different wine samples.

摘要

提出了一种快速有效的微萃取技术,用于在气相色谱串联质谱(GC-MS/MS)分析之前从葡萄酒样品中预浓缩 2,4,6-三氯苯甲醚(2,4,6-TCA)。所提出的技术基于超声处理(US),以促进萃取阶段的乳化现象。研究并优化了影响目标分析物相对响应的几个变量。在最佳实验条件下,定量提取了 2,4,6-TCA,实现了增强因子(EF)>或= 400 和检测限(LOD)0.6-0.7 ng L(-1),相对标准偏差(RSD)<或= 11.3%,当分析 10 ng L(-1) 2,4,6-TCA 标准-葡萄酒样品混合物时。白葡萄酒和红葡萄酒的校准曲线在 5-1000 ng L(-1)范围内呈线性,估计系数(r(2))>或= 0.9995。通过在两个浓度(10 和 50 ng L(-1))进行标准加入法验证了该方法的有效性,回收率>80%,表明该方法具有令人满意的稳健性。该方法成功应用于不同葡萄酒样品中 2,4,6-TCA 的测定。

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