Application of solid-phase microextraction and gas chromatography-mass spectrometry for the determination of chlorophenols in leather.
Application of solid-phase microextraction and gas chromatography-mass spectrometry for the determination of chlorophenols in leather.
复制标题
DOI：
10.1002/jssc.201100726
复制
发表时间：
2012-02
影响因子：
3.1
通讯作者：
C. D. de Souza Silveira;Edmar Martendal;V. Soldi;E. Carasek
中科院分区：
文献类型：
--
作者：
C. D. de Souza Silveira;Edmar Martendal;V. Soldi;E. Carasek
建立了顶空固相微萃取（HS-SPME）-气相色谱-选择离子监测-质谱（GC-SIM-MS）联用技术测定皮革样品中16种酚类化合物的分析方法。以聚丙烯酸酯85 μm（PA）为原料，采用两水平析因设计和中心复合设计，对HS-SPME的工艺条件进行了优化。最佳提取条件为：200 μL衍生剂（乙酸酐）、20 mL饱和NaCl水溶液、提取时间50 min、提取温度75°C。在固定皮革样品质量（250 mg）、小瓶体积（40 mL）、磷酸盐缓冲液pH（12）和浓度（50 mmol/L）的条件下，得到了所有优化条件。方法的检出限为0.03 ~ 0.20 ng/g，相对标准偏差（RSD）小于10.23%（n=6），线性范围为800 ng/g（氯酚）和1325 ng/g（2-苯基苯酚）。通过在皮革样品中加入不同量的酚类物质，在三个浓度水平下研究了回收率，得到了90.0 - 107.2%的良好回收率。该方法简单、快速、灵敏，适用于皮革样品中酚类物质的定量分析。
This paper proposes a new analytical procedure based on the headspace solid-phase microextraction (HS-SPME) technique and gas chromatography-selected ion monitoring-mass spectrometry (GC-SIM-MS) for the determination of 16 phenols extracted from leather samples. The optimized conditions for the HS-SPME were obtained through two experimental designs - a two-level fractional factorial design followed by a central composite design - using the commercial SPME fiber polyacrylate 85 μm (PA). The best extraction conditions were as follows: 200 μL of derivatizing agent (acetic anhydride), 20 mL of saturated aqueous NaCl solution and extraction time and temperature of 50 min and 75°C, respectively. All optimized conditions were obtained with fixed leather sample mass (250 mg), vial volume (40 mL) and phosphate buffer pH (12) and concentration (50 mmol/L). Detection limits ranging from 0.03 to 0.20 ng/g, and relative standard deviation (RSD) lower than 10.23% (n=6) for a concentration of 800 ng/g (chlorophenols) and 1325 ng/g (2-phenylphenol) in the splitless mode were obtained. The recovery was studied at three concentration levels by adding different amounts of phenols to the leather sample and excellent recoveries ranging from 90.0 to 107.2% were obtained. The validated method was shown to be suitable for the quantification of phenols in leather samples, as it is simple, relatively fast and sensitive.