A multiresidue method for determining 136 pesticides and metabolites in fruits and vegetables: Application of macroporous diatomaceous earth column

2020 ◽  
Vol 15 (3) ◽  
Author(s):  
S.-H. Tseng ◽  
Y.-J. Lin ◽  
H.-F. Lee ◽  
S.-C. Su ◽  
S.-S. Chou ◽  
...  
Keyword(s):  
Diatomaceous Earth ◽  
Fruits And Vegetables ◽  
Multiresidue Method

Applicability of a Carbamate Insecticide Multiresidue Method for Determining Additional Types of Pesticides in Fruits and Vegetables

1983 ◽  
Vol 66 (2) ◽  
pp. 234-240 ◽  
Author(s):  
Richard T Krause ◽  
E Michael August
Keyword(s):  
Liquid Chromatography ◽  
High Performance ◽  
Fruits And Vegetables ◽  
Naphthalene Acetic Acid ◽  
Gas Liquid Chromatography ◽  
Fluorescence Detector ◽  
Liquid Chromatograph ◽  
Multiresidue Method ◽  
Oxygen Analog ◽  
Azinphos Methyl

Abstract Several fruits and vegetables were fortified at a low (0.02-0.5 ppm) and at a high (0.1-5 ppm) level with pesticides and with a synergist, and recoveries were determined. Analyses were performed by using 3 steps of a multiresidue method for determining N-methylcarbamates in crops: methanol extraction followed by removal of plant co-extractives by solvent partitioning and chromatography with a charcoal-silanized Celite column. Eleven compounds were determined by using a high performance liquid chromatograph equipped with a reverse phase column and a fluorescence detector. Twelve additional compounds were determined by using a gas-liquid chromatograph equipped with a nonpolar packed column and an electron capture or flame photometric detector. Recoveries of 10 pesticides (azinphos ethyl, azinphos methyl, azinphos methyl oxygen analog, carbaryl, carbof uran, naphthalene acetamide, naphthalene acetic acid methyl ester, napropamide, phosalone, and phosalone oxygen analog) and the synergist piperonyl butoxide, which were determined by high performance liquid chromatography, averaged 100% (range 86-117) at the low fortification level and 102% (range 93-115) at the high fortification level. Quantitative recovery of naphthalene acetamide through the method required that an additional portion of eluting solution be passed through the charcoal column. Recoveries of 7 additional pesticides (dimethoate, malathion, methyl parathion, mevinphos, parathion, phorate oxygen analog, and pronamide), which were determined by gas-liquid chromatography (GLC), averaged 108% (range 100-120) at the low fortification level and 107% (range 99-122) at the high fortification level. DDT, diazinon, dieldrin, phorate, and pirimiphos ethyl, which were determined by GLC, were not quantitatively recovered.

scholarly journals Development and Validation of a Multiresidue Method for the Determination of Neonicotinoid and Macrocyclic Lactone Pesticide Residues in Milk, Fruits, and Vegetables by Ultra-Performance Liquid Chromatography/MS/MS

2010 ◽  
Vol 93 (2) ◽  
pp. 389-399 ◽  
Author(s):  
Alaa Kamel ◽  
Yaorong Qian ◽  
Elizabeth Kolbe ◽  
Charles Stafford
Keyword(s):  
Liquid Chromatography ◽  
Macrocyclic Lactone ◽  
Fruits And Vegetables ◽  
Ultra Performance Liquid Chromatography ◽  
Multiresidue Method ◽  
Target Analytes ◽  
Neonicotinoid Pesticides ◽  
Development And Validation ◽  
Concentration Levels

Abstract A multiresidue method was developed and validated for the determination of 13 neonicotinoid pesticides and metabolites, and nine macrocyclic lactone pesticides and veterinary drugs using SPE and ultra-performance liquid chromatography/MS/MS. The method was validated in milk, orange, spinach, apple, plum, watermelon, green bean, zucchini, broccoli, strawberry, grape, and tomato by analyzing replicates of residue-free control samples fortified with a mixture of 22 target analytes at three concentration levels. The recoveries of the analytes from the fortified matrixes were mostly within 70120, except for some of the neonicotinoid metabolites. The LOD values varied by analyte and matrix and ranged between 0.0012 ng/g. The developed method was successful in combining two widely different classes of compounds into a single analysis.

Modification of AOAC Multiresidue Method for Determination of Synthetic Pyrethroid Residues in Fruits, Vegetables, and Grains. Part I: Acetonitrile Extraction System and Optimization of Florisil Cleanup and Gas Chromatography

1995 ◽  
Vol 78 (6) ◽  
pp. 1481-1488 ◽  
Author(s):  
Guo-Fang Pang ◽  
Yan-Zhong Chao ◽  
Chun-Lin Fan ◽  
Jin-Jie Zhang ◽  
Xue-Min Li ◽  
...  
Keyword(s):  
Gas Chromatography ◽  
Fruits And Vegetables ◽  
Electron Capture Detection ◽  
Synthetic Pyrethroids ◽  
Capillary Gc ◽  
Pyrethroid Insecticides ◽  
Multiresidue Method ◽  
Polished Rice ◽  
The Individual

Abstract We present a multiresidue method for determination of synthetic pyrethroids in fruits, vegetables, and grains. The method is a modification of AOAC Method 970.52. Residues are extracted with acetonitrile (for fruits and vegetables) or acetonitrile–water (2 + 1) (for grains) and then transferred to hexane. Coextractives are removed by acetonitrile partitioning and open-column chromatography with deactivated Florisil. The final extract is analyzed by gas chromatography with electron capture detection (GC–ECD). An HP-17 wide-bore column is used to determine the total isomeric content of each insecticide, and a DB-5 narrow-bore column is used to determine the individual isomeric contents of each insecticide. The method was used to recover 8 pyrethroids (biphenthrin, fenpropathrin, cyhalothrin, permethrin, cypermethrin, fluvalinate, fenvalerate, and deltamethrin) spiked at 0.01–4.0 mg/kg in 20 crops (apple, pear, peach, banana, grape, strawberry, potato, tomato, cucumber, pepper, cabbage, carrot, celery, polished rice, wheat, green gram, buckwheat, sorghum, maize, and barley). Recoveries of the 8 pyrethroid insecticides in 6 crops ranged from 83.8 to 112.8%, with a coefficient of variation (CV) of 2.00 to 12.09% for the narrow- bore capillary GC (n = 6) and from 82.8 to 106.4%, CV = 2.93–12.19%, for the wide-bore capillary GC (n = 6). The minimum detectable levels of 0.004–0.028 mg/kg (for fruits and vegetables) or 0.01–0.08 mg/kg (for grains) for the 8 pyrethroids are easy to detect.

Modification of AOAC Multiresidue Method for Determination of Synthetic Pyrethroid Residues in Fruits, Vegetables, and Grains. Part II: Acetone Extraction System

1995 ◽  
Vol 78 (6) ◽  
pp. 1489-1496 ◽  
Author(s):  
Guo-Fang Pang ◽  
Yan-Zhong Chao ◽  
Chun-Lin Fan ◽  
Jin-Jie Zhang ◽  
Xue-Min Li ◽  
...  
Keyword(s):  
Fruits And Vegetables ◽  
Limit Of Detection ◽  
Water Extraction ◽  
Multiresidue Analysis ◽  
Pyrethroid Insecticides ◽  
Multiresidue Method ◽  
Extraction Solvent ◽  
Acetone Water ◽  
Coefficients Of Variation ◽  
Extraction Solvents

Abstract To optimize conditions and to evaluate further a multiresidue method for pyrethroids, various extraction solvents and partitioning conditions were examined. Acetone and acetonitrile (for fruits and vegetables) and acetone–water and acetonitrile–water (for grains) were used as solvents with or without acetonitrile partitioning. Twenty crops fortified with 8 pyrethroid insecticides at low, medium, and high levels were analyzed. For limit of detection (LOD) levels, repeatability tests were completed with acetone–water as extraction solvent. Recoveries of 8 pyrethroid insecticides at LOD levels were 76.2–99.6%, with coefficients of variation (CVs) of 2.08–10.90% for narrow-bore capillary gas chromatography (GC) (n = 6) and 80.1–107.3% with CVs of 3.76–15.38% for wide-bore capillary GO (n = 6). Both acetone or acetone–water extraction with acetonitrile partitioning and acetonitrile or acetonitrile–water extraction with acetonitrile partitioning are suitable for multiresidue analysis of pyrethroid insecticides. However, acetonitrile and acetonitrile– water as extraction solvents were better than acetone and acetone–water at LOD-fortified levels. This finding was confirmed chromatographically with pear, cucumber, and barley control samples.

Fast and Versatile Multiresidue Method for the Analysis of Botanical Insecticides on Fruits and Vegetables by HPLC/DAD/MS

2005 ◽  
Vol 53 (22) ◽  
pp. 8644-8649 ◽  
Author(s):  
Pierluigi Caboni ◽  
Giorgia Sarais ◽  
Alberto Angioni ◽  
Vincenzo Luigi Garau ◽  
Paolo Cabras
Keyword(s):  
Fruits And Vegetables ◽  
Botanical Insecticides ◽  
Multiresidue Method
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