气相色谱-二级质谱法测定木竹藤草制品中五氯苯酚

Determination of Pentachlorophenol in Wood, Bamboo,Cane and Grass Product by GC-NCI-MS/MS

研究建立了气相色谱-负化学电离源二级质谱法测定木竹藤草制品中五氯苯酚的方法.样品经甲醇萃取,在碳酸钾溶液中进行衍生法反应,五氯苯酚乙酰化衍生物用正己烷萃取,采用3对离子对(m/z308/265,m/z 308/231,m/z 308/202)同时监测,进行定性确证,选择丰度较高的离子对m/z 308/265为定量分析的离子对.结果表明:该方法灵敏度高,选择性好,回收率为92.8%~99.7%,相对标准偏差(RSD)1.23%~6.09%.五氯苯酚在0.002~1mg/L范围内线性关系良好;检出限为0.001mg/kg,能很好地满足复杂基体木竹藤草制品中五氯苯酚的测定.

In this paper, a method was established to determine Pentachlorophenol in wood, bamboo, cane and grass product by gas chromatography-negative chemical ionization tandem mass spectrometry(GC-NCI-MS/MS). The samples were extracted with methanol, and the extract is derivatized with acetic anhydride in potassium carbonate media, and then extracted with hexane. The derivative was detected qualitatively by GC-NCI-MS/MS with three ion pairs monitoring(m/z308/265, m/z 308/231, m/z 308/202)simultaneously and detected quantitatively with ion pair m/z 308/265(higher abundance). The linear relation is fine in the range of 0.002~1 mg/L, and the minimum detection limit, recoveries and the relative standard deviation are 0.001 mg/kg, 92.8% ~99.7% and 1.23%~6.09%, respectively.