Collaborative Study of the Ethyl Acetate Extraction, Sweep Co-distillation Cleanup, and GLC Determination, Using Six Parent Organophosphate Pesticides

1968 ◽  
Vol 51 (3) ◽  
pp. 662-665 ◽  
Author(s):  
R W Storherr ◽  
R R Watts

Abstract Nine chemists in five laboratories collaborated in testing the combined rapid ethyl acetate extraction and sweep co-distillation cleanup method for multiple organophosphate pesticide residues in crops. Pesticides were detected by GLC with the potassium thermionic detector. The six pesticides studied were Diazinon, methyl parathion, malathion, parathion, ethion, and carbophenothion. Six crops—kale, carrots, lettuce, apples, potatoes, and strawberries—were divided into three groups, and each laboratory was selected to work with a specific group. With unknown fortification levels of 1.0 and 0.5 ppm, the collaborators obtained recoveries of 90+% at each level.

1965 ◽  
Vol 48 (6) ◽  
pp. 1154-1158
Author(s):  
R W Storherr ◽  
R R Watts

Abstract A simple sweep co-distillation method which uses the Storherr tube was developed for cleanup of 2 g or less of crude crop extracts which contain organophosphate pesticide residues. Five crops (kale, carrots, apples, strawberries, and potatoes) were fortified at levels of 1.0, 0.5, and 0.1 ppm with a mixture containing Trithion, diazinon, malathion, methyl parathion, and parathion. The sweep co-distillation method was compared with the adsorption column method by use of this mixture. The range of average per cent recoveries were 89–101% and 83–96%, respectively. The cleanup required approximately 20 minutes per sample and was as good as, and in many cases better than, adsorption column chromatography. Detection of the organophosphate pesticides was performed by GLC with the thermionic detector.


1969 ◽  
Vol 52 (4) ◽  
pp. 811-817
Author(s):  
Raymond J Gajan

Abstract Ten laboratories collaboratively studied several single sweep oscillopolarographic methods designed to be used as confirmative procedures for several organophosphorus pesticide residues determined by GLC. Polarographic methods for the detection and determination of parathion, methyl parathion, diazinon, and/or malathion at 0.5 and 2.0 ppm in extracts of apples and lettuce were included in this study. All 10 laboratories successfully detected the organophosphorus pesticide residues and quantitative results were reported by seven laboratories. These results show that the polarographic methods can be used for rapidly confirming results obtained by the multiple detection procedures now in use.


2020 ◽  
Vol 4 (2) ◽  
pp. 98-110
Author(s):  
Widia Purnamasari ◽  
Moch Irfan Hadi ◽  
Eva Agustina

Excessive use of organophosphate pesticides is becoming more common these days. This can affect the level of pesticide residues in farmers' crops. Excessive spraying of pesticides can result in environmental pollution both small and large scale. If excessive exposure to these pesticides can cause damage to the ecosystem. The purpose of this study was to determine the level of organophosphate pesticide residues found in horticulture plants. This research method is a systematic review, by analyzing various studies regarding the contamination of organophosphate pesticide residues in horticultural crops. There are 20 studies from within the country. The results obtained in the form of levels of pesticide residues that are still below the threshold of the BMR (Maximum Residue Limit) of pesticides determined by SNI. Two other studies show that no pesticide residue content was detected. Conclusion: This shows that the sample tested is still safe for consumption. Socialization and education about the doses of pesticide use and how to reduce levels of pesticides in horticultural crops are needed to reduce the risk of exposure to pesticides


2019 ◽  
Vol 22 (2) ◽  
pp. 103
Author(s):  
Chrisna Adhi Suryono ◽  
Agus Sabdono ◽  
Subagiyo Subagiyo

Organophosphate pesticides were widely used in agriculture and OPP which was less accumulative and degradable but It has been found in an aquatic environment. The purpose of this study was to determine the level of organophosphate pesticide residues in bivalve which was fishing in North Coast of Java specifically the Demak and Surabaya.  Bivalvia, sediment and seawater samples were analysed using GC-MS. The results showed that the bivalves of A inaequivalvis, P viridis, A pectinata captured in Demak and Surabaya were contaminated with organophosphate pesticide of chlorpyrifos, fenitrothion and profenofos. The chlorpyrifos was found in all species of bivalves, but the highest concentrations of OPP were profenophos> chlorpyrifos > fenitrothion respectively. ANOVA test results show that there was a very significant difference in OPP residues in bivalves p = 0.009, but there was no difference in OPP residues between locations.Organoposfat pestisida (OPP) banyak digunakan secara meluas dalam pertanian dan OPP tersebut kurang akumulatif dan mudah terurai namun keberdaanya telah di temukan dala lingkungan perairan. Tujuan dari penelitian adalah untuk mengetahui tingkat akumulasi residu pestisida organoposfat yang terdapat di bivalvia yang ditangkap di pesisir Utara Jawa khususnya wilayah Demak dan Surabaya.  Sampel bivalvia, sedimen dan air laut dianalisa menggunakan GC-MS. Hasil penelitian menunjukan bahwa bivalvia A inaequivalvis, P viridis, A pectinata yang ditangkap di Demak dan Surabaya terkontaminasi pestisida organoposfat jenis Klorpirifos, Fenitrotion dan Profenofos. Klorpirifos ditemukan pada semua bivalvia, namun konsentrasi tertinggi OPP secara berurutan profenofos > klorpirifos > fenitrotion.  Hasil uji ANOVA  menunjukan adanya perbedaan yang sangat nyata residu OPP dalam bivalvia p= 0.009,  namun tidak ada berbedaan residu OPP antar wilayah lokasi.


Recently, the appearance of pesticide residues into the environment poses serious risks to the living organisms. In this view, we explored a novel and superior photocatalyst based on nanostructured sphere-like nickel tungstate (NiWO4 NSs) for the degradation of organophosphate pesticide methyl parathion (MP) under visible light irradiation, for the first time. The NiWO4 NSs were tailored through simple precipitation technique and confirmed by several spectroscopic techniques. Fascinatingly, the NiWO4 NSs portrayed superior photodegradation performances towards MP degradation with superior stability.


1967 ◽  
Vol 50 (2) ◽  
pp. 430-439
Author(s):  
John R Wessel

Abstract Twelve collaborators from 6 laboratories studied a multiple detection gas chromatographic method (potassium chloride thermionic plus electron capture) for ronnel, ethion, Trithion, diazinon, methyl parathion, parathion, and malathion in leafy vegetables (lettuce) and fruits (apples). Residues were present at the 0.5 and 5.0 ppm levels. Average recoveries for the 7 residues at the 0.5 ppm level were 88.7% (by thermionic) and 91.2% (by electron capture) from apples. At the 5.0 ppm level, average recoveries were 89.0% (by thermionic) and 89.4% (by electron capture) from lettuce. Residues in most instances were confirmed by TLC.


2008 ◽  
Vol 91 (1) ◽  
pp. 202-236 ◽  
Author(s):  
Kathleen D Miller ◽  
Paul Milne ◽  
B Berry ◽  
B Loo ◽  
P Matteini ◽  
...  

Abstract A collaborative study was conducted on a method for the measurement of 19 low-level pesticide residues in soft drinks and sports drinks by gas chromatography with mass spectrometry (GC/MS). The pesticide residues determined were 2,4-dichlorodiphenyldichloroethylene (2,4-DDE); 2,4-dichlorodiphenyldichloroethane (2,4-DDD); 4,4-dichlorodiphenyldichloroethylene (4,4-DDE); 2,4-dichlorodiphenyltrichloroethane (2,4-DDT); 4,4-dichlorodiphenyltrichloroethane (4,4-DDT); 4,4-dichlorodiphenyldichloroethane (4,4-DDD); -endosulfan; endosulfan-sulfate; dieldrin; aldrin; ethion; chlorpyrifos; -endosulfan; malathion; methyl-parathion; -hexachlorocyclohexane (-HCH); -HCH; -HCH; and -HCH. Blind fortification solutions containing 4 different levels of pesticide residues (0, 0.1, 0.5, and 1.0 g/L) were provided to 8 collaborating laboratories who used them to create test samples in 6 matrixes (also provided): 2 colas, a diet cola, a clear lemon-lime soft drink, an orange soft drink, and a sports drink. Reproducibility (RSDR) for all 19 pesticide residues in all matrixes ranged from 7 to 151 at the 0.1 g/L level, 11 to 121 at 0.5 g/L, and 14 to 67 at 1.0 g/L. Repeatability (RSDr), applicable to the diet cola and the sports drink, ranged from 1 to 76 for the 19 pesticide residues at the 0.1 g/L level, 9 to 38 at 0.5 g/L, and 9 to 38 at 1.0 g/L. Recoveries for the 19 pesticide residues in allmatrixes ranged from 77 to 645 at the 0.1 g/L level, 60 to 231 at 0.5 g/L, and 61 to 146 at 1.0 g/L. It is recommended that the method be accepted by AOAC as Official First Action with a limit of quantification (LOQ) equal to 0.5 g/L for 4,4-DDT; 2,4-DDT; 2,4-DDD; 4,4-DDE; 4,4-DDD; 2,4-DDE; aldrin; dieldrin; -endosulfan; endosulfan-sulfate; chlorpyrifos; and ethion, and an LOQ equal to 1.0 g/L for -endosulfan; -HCH; -HCH; -HCH; -HCH; methyl-parathion; and malathion.


1965 ◽  
Vol 48 (6) ◽  
pp. 1158-1160
Author(s):  
Randall R Watts ◽  
Robert W Storherr

Abstract An ethyl acetate extraction method for organophosphate pesticide residues on crop samples requires about 40 minutes for extraction and preparation of sample. This procedure eliminates the lengthy acetonitrile concentration and reduces the volume of solvent used in the acetonitrile procedure. Dimethoate, diazinon, Trithion, Guthion, Phosdrin, and parathion were easily extracted from field-sprayed kale by the ethyl acetate extraction method.


2016 ◽  
Vol 44 (1) ◽  
pp. 1-8
Author(s):  
Maria Zaman ◽  
Nasim Sultana ◽  
Mozaffar Husain ◽  
M Niamul Naser

Pesticide residues, specially the persistent organic pollutant (POP) were analyzed from some fish species of Rangpur floodplain, Bangladesh. Fish samples were extracted with ethyl acetate, cleaned by sulphuric acid and analyzed by gas chromatograph and gas chromatograph-mass spectrometer. Presence of endrin was detected in Taki fish (Channa punctatus) samples. Traces of other pesticides were also evident. This confirms the use of banned pesticide in the northwestern Bangladesh. We discussed some consequences of public health issues if these contaminantspasses through in the higher food chain from the wetland ecosystem.Bangladesh J. Zool. 44(1): 1-8, 2016


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