摘要
研究并建立了测定贝类中多氯联苯残留的气相色谱-串联质谱(GC—MS/MS)方法。通过正己烷和丙酮的混合溶液超声提取,硅胶柱净化,旋转蒸发浓缩,采用GC—MS/MS多反应监测(MRM)方式测定,可同时对贝类中的7种指示性多氯联苯进行定性和定量。研究结果表明:7种指示性多氯联苯的检出限(S/N=3)为0.0066~0.0098μg/kg,定量限(S/N=10)为0.02μg/kg;在0.1~50.0ng/mL时峰强度与质量浓度的线性关系良好(r〉0.99)。方法的平均回收率为73%~113%。该法简便快捷,降低了分析成本,在一定程度上实现了持久性污染物的快速检测和确证。
A method for determining residues of seven polychlorinated biphenyls (7 PCBs) in seashell was developed by gas chromatography-tandem mass spectrometry. The sample was extracted with blended solution of hexane and acetone, cleaned-up by column of silica gel, and concentrated with a rotary evaporator. The mass spectrometer was operated using multiple reaction monitoring (MRM)for qualitative and quantitative analysis of 7 PCBs in seashell at the same time. The results showed that the limits of detection for 7 PCBs were 0. 0066- 0. 0098 μg/kg (S/N= 3), and the limits of quantitation were 0.02 μg/kg (S/N=10). The method was linear over the range from 0.1 ng/mL to 50 ng/mL with correlation coefficients 〉0. 99, and the average recoveries for 7 PCBs were between 73% and 113%. The method is simple, fast and low cost, which facilitates the fast analysis of the permanent contaminations.
出处
《分析科学学报》
CAS
CSCD
北大核心
2009年第6期647-651,共5页
Journal of Analytical Science
基金
农业部948资助项目(No.2006G56)
国家科技支撑计划项目(No.2007BAD62B02)
国家863计划项目(No.2008AA100805)
关键词
多氯联苯
贝类
气相色谱-串联质谱法
Polychlorinated biphenyls
Seashell
Gas chromatography-tandem mass spectrometry