Determination of Different Polarity Pesticide Residues in Water by Solid Phase Membrane Extraction-Ultrasonic Assisted Elution-in Situ Derivatization Method

• Published in: Fēnxī huàxué 2014-01, Vol.42 (4), p.592-596
• Main Authors: ZHANG, Li, GUI, Jian-Ye, ZHAO, Guo-Xing, TIAN, Lai-Sheng, ZHANG, Yong-Tao, LI, Xiao-Yao, ZHANG, Chen-Ling
• Format: Article
• Language: chi ; eng
• Subjects: Herbicides; Insecticides; Ionization; Mass spectrometry; Membranes; Polarity; Recovery; Solid phases
• ISSN: 0253-3820
• DOI: 10.3724/SP.J.1096.2014.30833

A method was developed for the determination of polar herbicides and nonpolar insecticides by solid phase membrane extraction-ultrasonic assisted elution-in situ derivatization-gas chromatography-negative chemical ionization mass spectrometry. Two kinds of organic compounds were extracted by using C sub(8) membrane at pH 3 in 1000 mL water sample within 10 min. Then herbicides were derivatized and eluted simultaneously, with insecticides being eluted under ultrasonic effect within 30 min. The objectives were separated in a HP-5MS (30 m X 0. 25 mm X 0.25 mu m) column, and then detected by negative chemical ionization mass spectrometry in 10 min. The derivatization reaction between acid herbicides and derivatization reagent was specific reaction with functional groups. In addition, reaction time was fairly short, so that the insecticide recovery was good. The experiment results showed that there was a good linear relationship in the range of 10 mu g/L-250 mu g/L with correlation coefficients higher than 0.9978. The detection limits were less than 1.0 mu g/L. The spiked recoveries of different matrices and different concentrations varied from 88% to 107% with relative standard deviations between 3.6% and 9.7%.