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通过双搅拌棒吸附萃取-热脱附-低质量热气相色谱-质谱联用技术快速筛查水样中的农药多残留

Fast screening of pesticide multiresidues in aqueous samples by dual stir bar sorptive extraction-thermal desorption-low thermal mass gas chromatography-mass spectrometry.

作者信息

Ochiai Nobuo, Sasamoto Kikuo, Kanda Hirooki, Nakamura Sadao

机构信息

Gerstel K.K., 2-13-18 Nakane, Meguro-ku, Tokyo 152-0031, Japan.

出版信息

J Chromatogr A. 2006 Oct 13;1130(1):83-90. doi: 10.1016/j.chroma.2006.06.032. Epub 2006 Jun 30.

Abstract

A method for fast screening of pesticide multiresidues in aqueous samples using dual stir bar sorptive extraction-thermal desorption-low thermal mass gas chromatography-mass spectrometry (dual SBSE-TD-LTM-GC-MS) has been developed. Recovery of 82 pesticides - organochlorine, carbamate, organophosphorous, pyrethroid and others - for the SBSE was evaluated as a function of octanol-water distribution coefficients (log K(o/w): 1.7-8.35), sample volume (2-20 mL), salt addition (0-30% NaCl), and methanol addition (0-20%). The optimized method consists of a dual SBSE performed simultaneously on respectively a 20-mL sample containing 30% NaCl and a 20-mL sample without modifier (100% sample solution). One extraction with 30% NaCl is mainly targeting solutes with low K(o/w) (log K(o/w)<3.5) and another extraction with unmodified sample solution is targeting solutes with medium and high K(o/w) (log K(o/w)>3.5). After extraction, the two stir bars are placed in a single glass desorption liner and are simultaneously desorbed. The desorbed compounds are analyzed by use of LTM-GC-MS with fast temperature programming (75 degrees C min(-1)) using a 0.18 mm i.d. narrow-bore capillary column and fast scanning (10.83 scan s(-1)) using quadrupole MS. The method showed good linearity (r(2)>0.9900) and high sensitivity (limit of detection: <10 ng L(-1)) for most of the target pesticides. The method was applied to the determination of pesticides at nanograms per liter levels in river water and brewed green tea.

摘要

已开发出一种使用双搅拌棒吸附萃取-热脱附-低热质量气相色谱-质谱联用仪(双SBSE-TD-LTM-GC-MS)快速筛查水样中农药多残留的方法。评估了82种农药(有机氯、氨基甲酸酯、有机磷、拟除虫菊酯及其他农药)在搅拌棒吸附萃取中的回收率,该回收率是正辛醇-水分配系数(log K(o/w):1.7 - 8.35)、样品体积(2 - 20 mL)、加盐量(0 - 30% NaCl)和加甲醇量(0 - 20%)的函数。优化后的方法包括在分别含有30% NaCl的20 mL样品和未加改性剂的20 mL样品(100%样品溶液)上同时进行双搅拌棒吸附萃取。用30% NaCl进行的一次萃取主要针对低K(o/w)(log K(o/w)<3.5)的溶质,而用未改性样品溶液进行的另一次萃取则针对中高K(o/w)(log K(o/w)>3.5)的溶质。萃取后,将两根搅拌棒置于单个玻璃解吸衬管中并同时解吸。解吸后的化合物使用内径0.18 mm的窄口径毛细管柱通过快速程序升温(75℃ min(-1))的低热质量气相色谱-质谱联用仪进行分析,并使用四极杆质谱仪进行快速扫描(10.83次扫描 s(-1))。该方法对大多数目标农药显示出良好的线性(r(2)>0.9900)和高灵敏度(检测限:<10 ng L(-1))。该方法应用于测定河流水和冲泡绿茶中纳克每升水平的农药。

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