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PTV-GC/MSD同时测定环境水中57种农药残留 被引量:11

Determination 57 pesticide residues in environment water using PTV-GC/MS
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摘要 目的:建立一种同时测定环境水中57种农药残留的新方法.方法:采用C18和Sep-pak Porapak Rox固相萃取小柱联用提取、浓缩环境水中痕量农药,用气相色谱/质谱联用仪(GC/MSD)全扫描方式进行分析测定.在GC/MSD上用程序升温汽化进样器实施大体积进样,在毛细管柱上进样量为 40 μl.结果:各农药加标浓度为 0.01 mg/L 时,回收率在 74.5%~116.5% 之间,变异系数小于 7.8%.对各农药的检出限在 0.0001~0.01 mg/L 之间.结论:该方法简单快速、灵敏度高,完全能满足农药残留监控的要求. Objective:To set up a method for simultaneously determining 57 pesticides in environment water. Methods:Conventional liquid - liquid extract was displaced by solid phase extract using C18 and Sep - pak Porapak Rox SPE cartridge to extract and clean the pesticide residues from environment water. The pesticides were determined by gas chromatography with mass selective detection in scan model. Programmed temperature vaporization (PTV) large volume injector (LVI) was applied to inject the sample. By optimizing of PTV large - volume injection, the total injection volume reached 40 μl which was 40 times of ordinary injection volume. Results:The rates of recovery ranged from 74. 5% to 116.5% with relative standard deviation lower than 7.8% when the spiked level of the pesticide residues was 0. 01 mg/L The detection limits of the pesticides were 0. 0001 -0. 01 mg,/L. Conclusion:The method is sensitive and simple and meets the determinative requirement of pesticide residues.
出处 《中国卫生检验杂志》 CAS 2005年第9期1030-1032,共3页 Chinese Journal of Health Laboratory Technology
基金 广东省科技项目2004A304001的支持
关键词 程序升温汽化大体积进样 气相色谱/质谱 农药 固相萃取 Muhipesticide residues Programmed - temperature vaporization GC/MS Environment water
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参考文献3

  • 1Concha GE, Turnes CML Optimisation of a programmed spht - sphtless injector in the gas chromatographic - nmss spectrometric determination of organochlorine pesticides[J]. J Chromatgr A,2002,958( 1 -2) :17 -24.
  • 2I Vassilakis, D Tsipi, M Scoullos. Determination of a variety of chemical classes of pesticides in surface and ground waters by off - line solid- phase extraction, gas chromatography with electron - capture and nitrogen -phosphorus detection, and high -performance liquid chromatography with postcolumn derivatization and fluorescence detection [ J ].J Chromatogr A. 1998.823:49 - 58.
  • 3Pilar VA, Natalia C, Ignacto LPG, et al. Capillary gas chromatography with atomic emission detection for pesticide analysis in soil samples[J]. J Agric Food Chem,2003, 51, 3704-3708.

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