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发布者:鑫达医学翻译公司 发布时间:2011-07-10 8:50:52 阅读:

原文:
A method was developed to analyze 10 pyrethroid insecticides in sediment by gas chromatography-ion trap tandem mass spectrometry (GC–MS/MS) after accelerated solvent extraction and solid phase extraction cleanup. The MS/MS parameters included selection of the precursor and product ions, excitation mode, excitation amplitude and the stability parameter qz, and were optimized to maximize detection sensitivity. Due to its superior ability to remove background noise, GC–MS/MS showed elevated selectivity and improved confidence in peak identification compared to GC-electron capture detector (ECD). The instrumental detection limits for GC–MS/MS ranged from 148 to 4033 fg, and the calibration curves were linear from 5 to 1000g/L for all of the pyrethroids except cyfluthrin. The method detection limits for pyrethroids ranged from 0.10 to 0.80g/kg dry sediment, while the recoveries were 59.7–128%, 60.6–90.9% and 63.2–83.6% with the relative standard deviations of 5.3–25.3%, 1.1–10.6% and 3.0–15.6% at the spiking levels of 1, 5 and 20g/kg, respectively. Field sediment collected from California was used to validate the newly developed method, and analytical results were comparable to those by GC-ECD in most cases. However, as the result of a cleaner background, more pyrethroids were identified by GC–MS/MS.

译文:
本报道发明一种加速溶剂萃取(ASE)与固相萃取净化(SPE)后采用气相色谱/离子阱串联质谱 (GC–MS/MS) 分析沉积物内的10种拟除虫菊酯杀虫剂的方法。串联质谱(MS/MS)参数包括前体离子和产物离子、激发模式、激发振幅与稳定性参数qz,用以优化检测的最高灵敏度。GC–MS/MS具有清除本底噪音的超强性能,与气相色谱电子捕获检测器(GC-ECD)相比,其选择性较高,并可提高峰鉴定的置信度。GC-MS/MS的检出限为148~4033fg,除氟氯氰菊酯外其他9种拟除虫菊酯的校准曲线(5~1000μg/L范围内)均呈线性关系。 该方法对拟除虫菊酯的检出限为0.10~0.80μg/kg沉积物干样,1、5与20μg/kg加标水平下的恢复率分别为为59.7–128%、60.6–90.9%与63.2–83.6%,相对标准偏差分别为5.3–25.3%、1.1–10.6%与3.0–15.6%。采用美国加州获取的沉积物对该种新方法进行验证,多数情况下所得结果与GC-ECD所得结果相当。此外,GC-MS/MS所得本底更为清晰。因此,可检出更多的拟除虫菊酯。
 


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