固相萃取-气相色谱-串联质谱法测定木耳中五氯苯酚

Determination of pentachlorophenol in agaric by solid phase extraction coupled with gas chromatography-tandem mass spectrometry

中文关键词:  气相色谱质谱质谱法  五氯苯酚  木耳

英文关键词:gas chromatography-tandem mass spectrometry  pentachlorophenol  agaric

中文摘要:

      目的 建立固相萃取-气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry, GC-MS/MS)测定木耳中五氯苯酚的分析方法。方法 以2,4,6-三溴苯酚为内标物, 样品经5%三氯乙酸水溶液浸提, 以乙酸乙酯/正己烷液-液分配法萃取五氯苯酚, 经SLC(氧化铝/SCX)固相萃取柱净化样品提取液, 乙酸酐衍生, HP-5MS毛细管柱(30 m×0.25 mm, 0.25 μm)分离样品, 在多反应监测(multiple reaction monitoring, MRM)模式下, 采用内标法定量。结果 方法在五氯苯酚质量浓度1~100 ng/mL范围具有良好线性关系, 线性相关系数大于0.9999, 在方法线性范围内低、中、高3个浓度水平加标回收率在89.3%~108.7%之间, 相对标准偏差2.1%~9.0%。方法检出限为0.06 μg/kg, 定量限为0.20 μg/kg。结论 本方法灵敏度高, 方法稳定, 重现性好, 可用于木耳样品中五氯苯酚的定性定量测定。

英文摘要:

      Objective To establish an analytical methods for the pentachlorophenol in agaric by solid-extraction coupled with gas chromatography-tandem mass spectrometry (GC-MS/MS). Methods Using 2,4,6-tribromophenol as the internal standard, the agaric samples were extracted with 5% trichloroacetic acid aqueous solution, and pentachlorophenol was extracted using ethyl acetate/n-hexane liquid-liquid extraction method. The samples extracted liquid were purified using SLC (alumina/SCX) solid-phase extraction column, followed by acetic anhydride derivatization and separated by HP-5MS capillary column (30 m×0.25 mm, 0.25 μm), and detected in multiple reaction monitoring (MRM) mode and quantitated using an internal standards method. Results The method had a good linear relationship in the range of mass concentration of pentachlorophenol from 1 to 100 ng/mL, and the linear correlation coefficient was greater than 0.9999, the recoveries of the pentachlorophenol at the 3 spiked concentrations were 89.3%?108.7% and the relative standard deviations were 2.1%?9.0%. The limit of detection was 0.06 μg/kg, and the limit of quantitation was 0.20 μg/kg. Conclusion This method has high sensitivity, stability and good reproducibility, and can be used for qualitative and quantitative determination of pentachlorophenol in agaric samples.