金属-有机纳米管分散固相萃取-气相色谱-串联质谱高灵敏分析环境水样中痕量多氯联苯

采用含铅金属-有机纳米管为吸附剂,基于分散固相萃取和气相色谱-串联质谱建立了一种高灵敏分析环境水样中痕量多氯联苯的方法.采用正交设计响应面法对影响萃取效果的重要因素(如离子强度、萃取时间和吸附剂用量等)进行了优化.获得的最优条件为:离子强度4.92 %(w/V)NaCl,萃取时间4.5 min,正己烷为解吸剂,吸附剂用量62.5 mg.在优化条件下,方法的线性范围为2~1000 ng/L,检出限为0.26~0.82 ng/L. 日内和日间相对标准偏差分别为0.8%~5.5% (200 ng/L, n=6)和2.7%~7.4% (200 ng/L, n=6).将本方法应用于实际环境水样中多氯联苯的分析,回收率为78.9%~113.3%,结果满意.

Metal Organic Nanotubes-based Dispersive Solid Phase Extraction-Gas Chromatography-Tandem Mass Spectrometry for SensitiveAnalysis of Polychlorinated Biphenyls in Environmental Water Samples

A method of metal organic nanotubes-based dispersive solid phase extraction-gas chromatography-tandem mass spectrometry was developed for sensitive analysis of polychlorinated biphenyls in environmental water samples.Related important factors influencing enrichment efficiency, such as ionic strength, extraction time and amount of adsorbent, were investigated.Response surface methodology was used to optimize these factors in detail.Under the optimal conditions such as 4.92% (w/V) NaCl, 4.5 min of extraction time, 62.5 mg of adsorbent, and n-hexane as desorption solvent, wide linearity (2-1000 ng/L or 5-1000 ng/L), and low limits of detection (0.26-0.82 ng/L) were achieved.The intra-day and inter-day relative standard deviations were 0.8%-5.5% (200 ng/L, n=6)and 2.7%-7.4% (200 ng/L, n=6), respectively.Finally, this method was successfully applied to the sensitive analysis of 6 kinds of PCBs in environmental water samples, with satisfactory recoveries of 78.9%-113.3%.