Development of stir-bar sorptive extraction-thermal desorption-gas chromatography-mass spectrometry for the analysis of musks in vegetables and amended soils
Development of stir-bar sorptive extraction-thermal desorption-gas chromatography-mass spectrometry for the analysis of musks in vegetables and amended soils
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DOI：
10.1016/j.aca.2013.12.036
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发表时间：
2014-02-17
影响因子：
6.2
通讯作者：
Prieto, Ailette
中科院分区：
文献类型：
--
作者：
Aguirre, Josu;Bizkarguenaga, Ekhine;Prieto, Ailette
本研究旨在建立一种灵敏、环保的混合萃取-热解吸-气相色谱-质谱联用（dd - gc - ms）法测定蔬菜（生菜、胡萝卜和辣椒）和改良土壤样品中8种合成麝香（麝香香、麝香酮、牛油内酯、麝香内酯、galaxolide、phantolide、trasolide和羊绒）的方法。首先研究了顶空（HSSE）和浸没（SBSE）两种吸附萃取方式。在浸没模式下取得了最好的效果，并进行了进一步的研究。通过实验设计考察了甲醇（20%）和NaC1（0%）、萃取温度（40℃）和萃取时间（180 min）、萃取溶剂体积（9 mL）和搅拌速度（600 rpm）对SBSE萃取效率的影响。在TD的情况下，研究了解吸时间（10分钟）、解吸温度（300℃）、低温聚焦温度（30℃）、排气流量（75 mL/min）和排气压力（7.2 psi），采用了分数析因设计和中心复合设计（CCD）。在两种不同浓度水平下，对该方法进行了表观回收率（AR%）、方法检出限（MDLs）和精密度的验证。尽管在大多数情况下，使用仪器校准的定量结果不一致，但在采用基质匹配校准方法的情况下，在评估的两种浓度水平下，所有分析物和基质的回收率（74-126%）都令人满意。蔬菜和改良土壤样品的MDLs分别在0.01 ~ 0.8 ng/g和0.01 ~ 1.1 ng/g范围内。所有分析物和基质的RSD值均在1-23%之间。最后，将该方法应用于蔬菜和改良土壤样品中麝香的测定。(C) 2014 Elsevier B.V.版权所有
The aim of this study was to develop a sensitive and environment-friendly method based on stir-bar sorptive extraction (SBSE) followed by thermal desorption-gas chromatography-mass spectrometry (TD-GC-MS) to determine 8 synthetic musks (musk ambrette, musk ketone, celestolide, tonalide, galaxolide, phantolide, traseolide, and cashmeran) in vegetables (lettuce, carrot, and pepper) and amended soil samples. In a first step sorptive extraction was studied both in the headspace (HSSE) and in the immerse mode (SBSE). The best results were obtained in the immersion mode which was further studied. The influence of the main factors: methanol (20%) and NaC1 addition (0%), extraction temperature (40 C) and time (180 min), extraction solvent volume (9 mL) and stirring rate (600 rpm) on the efficiency of SBSE was evaluated by means of experimental designs. In the case of TD, desorption time (10 min), desorption temperature (300 C), cryo-focusing temperature ( 30 C), vent flow (75 mL/min) and vent pressure (7.2 psi) were studied using both a fractioned factorial design and a central composite design (CCD). The method was validated in terms of apparent recoveries (AR%), method detection limits (MDLs) and precision at two different concentration levels. Although quantification using instrumental calibration rendered odd results in most of the cases, satisfactory recoveries (74-126%) were obtained in the case of matrix-matched calibration approach for all of the analytes and matrices studied at the two concentration levels evaluated. MDLs in the range of 0.01-0.8 ng/g and 0.01-1.1 ng/g were obtained for vegetables and amended soil samples, respectively. RSD values within 1-23% were obtained for all the analytes and matrices. Finally, the method was applied to the determination of musks in vegetable and amended soil samples. (C) 2014 Elsevier B.V. All rights reserved.