Determination of Organotins in Aquatic Food by Gas Chromatography with Pulsed Flame Photometric Detection

Abstract A method based on gas chromatography (GC)-pulsed flame photometric detection (PFPD) was developed to determine the levels of organotins in aquatic food. After being purified by gel-permeation chromatography in ethyl actatetetrahydrofuran, the organotin compounds were derivatized by pentylmagnesium bromide. The derivative products were injected into the GC system and detected by PFPD (sulfur mode). The method was validated by analysis of the certified reference material and spiked samples. Recoveries of organotins ranged from 84.1 to 116.6 with relative standard deviation between 1.3 and 16.0 when spiked at levels of 2, 10, and 40 g/kg. The limits of detection varied from 0.1 to 1.2 g/kg for shellfish and 0.1 to 0.5 g/kg for fish. The proposed method was suitable for determining organotins in aquatic foods.

Download Full-text

Determination of Nitrogen- and Phosphorus-Containing Pesticide Residues in Vegetables by Gas Chromatography with Nitrogen–Phosphorus and Flame Photometric Detection after Gel Permeation Chromatography and a Two-Step Minicolumn Cleanup

Journal of AOAC International ◽

10.1093/jaoac/86.6.1241 ◽

2003 ◽

Vol 86 (6) ◽

pp. 1241-1251 ◽

Cited By ~ 5

Author(s):

Eiji Ueno ◽

Harumi Oshima ◽

Isao Saito ◽

Hiroshi Matsumoto

Keyword(s):

Gas Chromatography ◽

Pesticide Residues ◽

Gel Permeation Chromatography ◽

Good Resolution ◽

Photometric Detection ◽

Relative Standard ◽

Phosphorus Containing ◽

Gel Permeation ◽

Flame Photometric Detection ◽

Nitrogen Phosphorus

Abstract An efficient and reliable multiresidue method for determining pesticide residues in a large number of vegetable samples was studied. First, the important target compounds for monitoring, 52 nitrogen-and/or phosphorus-containing pesticides, were selected. The sample was extracted with acetonitrile, and the separated acetonitrile layer was cleaned up by a salting-out step. The acetonitrile extract was purified by gel permeation chromatography that divided the pesticide eluate into 2 fractions; the pesticide fractions were respectively purified by a 2-step minicolumn cleanup in which the second pesticide fraction was loaded on a silica-gel minicolumn. After a Florisil minicolumn was inserted on the silicagel minicolumn, the first pesticide fraction was loaded on the tandem minicolumn, which was eluted with acetone–petroleum ether (3 + 7). The combined eluate was subjected to dual-column gas chromatography (GC) with nitrogen–phosphorus and flame photometric detection. By application of the optimum cleanup conditions to the 52 pesticides selected, good resolution and low breakdown levels of the pesticides during GC were maintained. Recoveries of the 52 pesticides from fortified cabbage, lettuce, spring onion, and spinach ranged from 72 to 108% with relative standard deviations of 2–17%, except for the recoveries of methamidophos and chlorothalonil. The detection limits of the pesticides were satisfactory (0.001–0.009 mg/kg) for monitoring pesticide residues in vegetables.

Download Full-text

Determination of 49 Organophosphorus Pesticide Residues and Their Metabolites in Fish, Egg, and Milk by Dual Gas Chromatography–Dual Pulse Flame Photometric Detection with Gel Permeation Chromatography Cleanup

Journal of Agricultural and Food Chemistry ◽

10.1021/jf2043828 ◽

2012 ◽

Vol 60 (8) ◽

pp. 1906-1913 ◽

Cited By ~ 34

Author(s):

Lixin Yang ◽

Heli Li ◽

Fangang Zeng ◽

Yinping Liu ◽

Ruifeng Li ◽

...

Keyword(s):

Gas Chromatography ◽

Pesticide Residues ◽

Organophosphorus Pesticide ◽

Gel Permeation Chromatography ◽

Photometric Detection ◽

Gel Permeation ◽

Flame Photometric Detection

Download Full-text

Multiresidue Determination of Organophosphorus Pesticides in Ginkgo Leaves by Accelerated Solvent Extraction and Gas Chromatography with Flame Photometric Detection

Journal of AOAC International ◽

10.1093/jaoac/88.3.729 ◽

2005 ◽

Vol 88 (3) ◽

pp. 729-735

Author(s):

Xionghai Yi ◽

Yitong Lu

Keyword(s):

Gas Chromatography ◽

Solvent Extraction ◽

Solid Phase ◽

Organophosphorus Pesticides ◽

Accelerated Solvent Extraction ◽

Simple Method ◽

Photometric Detection ◽

Relative Standard ◽

Flame Photometric Detection

Abstract A rapid and simple method using accelerated solvent extraction and solid-phase extraction cleanup was developed and validated for the determination of 15 organophosphorus pesticides in ginkgo leaves by capillary gas chromatography with flame photometric detection. The pesticides were extracted at 100°C under 1500 psi pressure in <20 min. The average recovery from 10 g ginkgo leaves, fortified at 3 levels ranging from 0.05 to 1.00 mg/kg, was 95.2% with a relative standard deviation of 4.6%. The limits of detection ranged from 1.11 × 10−3 mg/kg (dimethoate) to 4.44 × 10−3 mg/kg (dichlorvos). The proposed method showed acceptable accuracy and precision while minimizing environmental concerns, time, and labor. Furthermore, the method could be easily applied to the monitoring of these 15 organophosphorus pesticides in ginkgo leaves.

Download Full-text

Determination of Tri-w-Butyltin and Di-/i-Butyltin Compounds in Fish by Gas Chromatography with Flame Photometric Detection

Journal of AOAC INTERNATIONAL ◽

10.1093/jaoac/71.2.360 ◽

1988 ◽

Vol 71 (2) ◽

pp. 360-363 ◽

Cited By ~ 2

Author(s):

Kumiko Sasaki ◽

Takashi Ishizaka ◽

Takashi Suzuki ◽

Yukio Saito

Keyword(s):

Gas Chromatography ◽

Gel Permeation Chromatography ◽

Mass Spectrometry Analysis ◽

Spectrometry Analysis ◽

Photometric Detection ◽

Flame Photometric Detection ◽

Methyl Derivatives ◽

Butyltin Compounds ◽

Good Agreement

Abstract An analytical method is described for the simultaneous quantitative determination of tri-n-butyltin and di-n-butyltin compounds in fish. The sample was extracted with 0.5N HCl-methanol, and the methanol solution was extracted with hexane. The extract was purified by gel permeation chromatography and treated with Grignard reagent to yield the methyl derivatives, which were determined by gas chromatography with flame photometric detection operated in the tin mode (610 nm). Recoveries of tri-n-butyltin chloride (Bu3SnCl) and di-n-butyltin dichloride (Bu2SnCl2) spiked to fish at the levels of 0.2 and 1.0 ppm ranged from 80 to 105%. Detection limits were 0.02 μg/g for both compounds. Tri-n-butyltin compounds equivalent to Bu3SnCl levels of 0.07-2.0 ppm and di-n-butyltin compounds equivalent to Bu2SnCl2 levels of 0.02-0.11 ppm were found in reared yellowtails, and these values showed good agreement with the results from gas chromatographic-mass spectrometry analysis.

Download Full-text

Determination of Polymerized Triglycerides in Frying Fats and Oils by Gel Permeation Chromatography: Interlaboratory Study

Journal of AOAC International ◽

10.1093/jaoac/77.3.667 ◽

1994 ◽

Vol 77 (3) ◽

pp. 667-671 ◽

Cited By ~ 6

Author(s):

Paul R Beljaars ◽

Remmelt Van Dijk ◽

Adrie A M Houwen-Claassen

Keyword(s):

Standard Deviation ◽

Relative Standard Deviation ◽

Gel Permeation Chromatography ◽

Fats And Oils ◽

Interlaboratory Study ◽

Frying Fats ◽

Relative Standard ◽

Gel Permeation ◽

Inspection Service

Abstract An interlaboratory study of the gel permeation chro-matographic (GPC) determination of polymerized triglycerides (PTG) in frying fats and oils was conducted by the Project Group on Collaborative Studies (PCS) of the Inspectorate for Health Protection, Food Inspection Service, The Netherlands. Thirteen laboratories participated in this study, which was focused on thermally abused oil and fat samples containing dimerized and polymerized triglycerides at levels just below and far above the Dutch regulatory limit of 16% (m/m). Samples were dissolved in tetrahydrofuran (THF) and analyzed on a GPC system, using THF as the mobile phase. Refractive index (Rl) detection was used to determine PTG. Six heat-processed fat samples containing from 14 to 28% (m/m) PTG at 3 different levels (3 pairs of split level samples) were single analyzed according to the proposed procedure. Data analysis was performed according to the International Union of Pure and Applied Chemistry/International Organization for Standardization/AOAC protocols for statistics. The results of 2 collaborators were identified as outliers at the 20% (m/m) PTG level by applying the paired Grubbs test at the 1% level of significance. The repeatability relative standard deviation (RSDr) values ranged from 0.48 to 2.25%, whereas the reproducibility relative standard deviation (RSDr) values ranged from 1.34 to 4.57%.

Download Full-text