Determination of organophosphorus pesticides by capillary electrophoresis‐inductively coupled plasma mass spectrometry with collective sample‐introduction technique

Abstract

A new method for the determination of organophosphorus pesticides using CE-ICP-MS with collective sample-introduction technique has been developed in this study. The method has been successfully used to separate and determine dimethoate, trichlorfon and glyphosate with an RSD of < 5% for migration times (n = 6) and < 4% for peak areas (n = 6). The experimental results showed that the collective sample-introduction considerably reduced the makeup volume and the dilution of analyte, and eventually resulted in a much lower detection limit and a much better electrophoretic resolution. The peak widths and the detection limits of dimethoate, trichlorfon and glyphosate obtained with this method are 15-17 s and 0.05-0.07 microg/mL (as compound), respectively. Using this method, we have successfully separated and determined dimethoate, trichlorfon and glyphosate in vegetable sample with a recovery of 90-96%.

Analysis of Phosphorus-containing Amino Acid-type Herbicides by Capillary Electrophoresis/Mass Spectrometry Using a Chemically Modified Capillary Having Amino Groups

“…Wuilloud et al 17) and Yang et al 18) analyzed these compounds using an untreated capillary with an alkaline BGE in positive-polarity mode. In these studies, the relative standard deviations (RSDs) of the migration times were relatively high (1.1-3.3%, 17) 4% 18) ). When a strong acidic BGE is used, EOF is suppressed, so that the electric current remains in negative-polarity mode.…”

“…RSDs of migration time were 0.36-0.52%, which were from 1/8 to 1/2 of the values obtained using untreated fused-silica capillaries. 18,19) The limits of detection (LODs), defined as a signal-to-noise ratio was 3 in extracted ion pherogram, were 0.5-10 µg/ml. When LODs in GC/MS methods were defined to be full-mass spectra measured, the LODs obtained using the proposed CE/MS method were 1/1000 (BIAL) -1 (AMPA) of the values obtained with N-methyl-N-(tert-butyldimethylsilyl)trifluoroacetamide derivatization, 2) although the values were higher than those obtained by GC/MS method (selected ion monitoring) with O-methyl, N-acetyl derivatization.…”

Analysis of Phosphorus-containing Amino Acid-type Herbicides by Sheathless Capillary Electrophoresis/Electrospray Ionization-Mass Spectrometry Using a High Sensitivity Porous Sprayer

“…Therefore, the EOF should be faster than their electrophoretic mobilities to detect them. [10][11][12] Combinations of formic acid with ammonia, diethylamine or ethylamine at various pHs and concentrations were examined. Migration times of GLYP, GLUF and BIAL were reasonably short and their peak shapes were better around pH 10.…”

Development and validation of a liquid chromatography–fluorescence–mass spectrometry method to measure glyphosate and aminomethylphosphonic acid in rat plasma

“…Thus, it is necessary to employ tedious and timeconsuming cleaning procedures, frequently involving the use of ion-exchange solvents [10][11][12][13][14] and further derivatization, in order to facilitate their chromatographic separation by gas GC [15,16], GC-MS [17][18][19][20][21], LC [3,[22][23][24][25][26] or LC-MS [27][28][29][30][31][32][33][34]. However, their low molecular mass and the effect of the phospholipid matrix also generate problems with LC-MS techniques, making it wiser to employ ionic chromatography and ICP-MS [35][36][37] or capillary electrophoresis coupled to ICP-MS [38]. Spectroscopy and other techniques have also been proposed as suitable methods to analyze these compounds [39][40][41][42][43].…”