自動前処理装置を用いるガスクロマトグラフィー : 負イオン化学イオン化質量分析法による除草剤の一斉分析(<特集>質量分析法の応用技術)

概要

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A method for the automatic analysis of 8 chlorinated phennoxy acid herbicides was developed using an automated sample preparation instrument in combination with a GC/MS with negative ion chemical ionization (NCI). The instrument can automate many sample preparation steps, such as solid phase extraction (SPE) and derivatization. All of the following steps were automated. 1) A sample of 10ml was injected into the SPE cartridge (THC) where 8 herbicides were retained. 2) The cartridge was then washed with dichloromethane. 3) The 8 herbicides were then eluated from the washed cartridge using 0.1% sulfuric acid-methanol (1ml). 4) The eluate was evaporated to dryness. 5) A derivatizing reagent, 2% pentafluorobenzyl bromide (PFBBr) in toluene and triethylamine, was added to the eluate. 6) And finally, the reaction mixture-sample solution was injected into the GC/MS by high pressure pulsed splitless injection. The total analysis time for 4 samples was approximately 4 hrs. The detection limits of the 8 herbicides ranged from 10ppt to 50ppt. The overall recoveries of the herbicides except for picloram were from 82 to 102% {RSD (n=5) were from 4.1 to 9.1%} for river water and from 96 to 116% {RSD (n=5) were from 4.3 to 7.3%} for wine, respectively. The recovery of picloram was about 50%, but we could get good results by using a standard calibration curve.
社団法人日本分析化学会の論文
1996-06-05