Column Extraction of Residues of Several Pesticides from Fruits and Vegetables: A Simple Multiresidue Analysis Method

1992 ◽  
Vol 75 (1) ◽  
pp. 53-61 ◽  
Author(s):  
Lajos Kadenczki ◽  
Zoltan Arpad ◽  
Ivan Gardi ◽  
Arpad Ambrus ◽  
Laszlo Gyorfi ◽  
...  

Abstract Homogeneous sample pulp, prepared from fruits and vegetables of different water content with or without additional water, Is adsorbed on the surface of activated Florisll to obtain a free-flowing powder, which is extracted In a glass column with ethyl acetate or methylene chloride-acetone (9 + 1, v/v). In most cases, no further cleanup Is necessary for subsequent gas chromatographic measurement. The recovery of pesticide residues, Including carbamate, organochlorlne, organophosphate, synthetic pyrethrold, triazlne, urea, and miscellaneous pesticides, Is generally ≥80%, and Is Independent of the sample material. The column extraction Is faster, less laborious, and less expensive than extractions based on traditional techniques, liquid partition, or other conventional chromatographic procedures.

1999 ◽  
Vol 82 (6) ◽  
pp. 1419-1435 ◽  
Author(s):  
Joanne Cook ◽  
Mary Pat Beckett ◽  
Brian Reliford ◽  
Walter Hammock ◽  
Marc Engel

Abstract Improved quality and efficiency of pesticide residue analysis were achieved by examining all aspects of the laboratory process. In an effort to eliminate methylene chloride hazardous waste, an acetonitrile extraction method, originally developed by the California Department of Agriculture, was modified and adopted. Sample size and solvent consumption were reduced with the new method. Custom glassware racks and disposable supplies reduced overall analysis time. Gravity-fed, solid-phase extraction simplified sample preparation and provided cleaner extracts for gas chromatographic analyses. Modifications to the method were made to achieve the ruggedness needed to maintain quality objectives during routine analysis. Instrumental improvements, including new selective detectors, retention time locking, and mass spectrometry screening for all samples, provided the laboratory with efficient, reliable, and confirmed analytical results.


Author(s):  
Fabiane M. Stringhini ◽  
Lucila C. Ribeiro ◽  
Graziela I. Rocha ◽  
Juliana D. de B. Kuntz ◽  
Renato Zanella ◽  
...  

AbstractTomato is well-known to be one of the most cultivated and consumed vegetables worldwide and frequently contain pesticide residues. Therefore, a simple multiresidue method was established and validated to determine 129 pesticides and metabolites in tomato samples using a modified acetate QuEChERS without cleanup for sample preparation and determination by ultrahigh-performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS). Dilution of the raw extract in different proportions of mobile phase was evaluated and a dilution of 10 times presented adequate results improving analysis performance while minimizing the matrix effect. Validation performed according to SANTE guideline presented satisfactory results. Practical method limit of quantification was 0.01 mg kg−1 for most compounds. Recoveries between 70 and 120% with precision ≤ 20% were found for most compounds and spike levels evaluated. Matrix effect results were not significant for most part of compounds. Method proved to be simple, robust, and effective to be applied in routine analysis. Method applicability was performed by analysis of samples commercialized in Brazil and positive results were found demonstrating the importance of the proposed method.


2012 ◽  
Vol 31 (3) ◽  
pp. 277-285 ◽  
Author(s):  
Young-Hwan Jeon ◽  
Jeong-In Hwang ◽  
Ji-Woon Ahn ◽  
Hyo-Young Kim ◽  
Jung-Ah Do ◽  
...  

Foods ◽  
2020 ◽  
Vol 9 (6) ◽  
pp. 746
Author(s):  
Kunho An ◽  
Inhwan Kim ◽  
Chan Lee ◽  
Joon-Kwan Moon ◽  
Hee-Jae Suh ◽  
...  

Morpholine salts of fatty acids have been used in wax coatings on the surfaces of fruit and vegetable commodities in China and the United States, etc. However, morpholine usage was prohibited in many other countries because of safety concerns. We optimized analytical methods to determine morpholine in the peel and pulp of fruits and vegetables by gas chromatography-mass spectrometry (GC-MS). This morpholine analysis method was applied to real samples of apples, citrus fruits, and vegetables from Korea, China, and the U.S. The method was validated using apple and citrus fruit peels and pulp. The method detection limit (MDL) was 1.3–3.3 µg/kg. The recovery rates of morpholine were 88.6–107.2% over a fortified level of 10–400 µg/kg. Intra-day and inter-day precisions were 1.4–9.4% and 1.5–2.8%, respectively. The morpholine concentrations were n.d. (not detected)–11.19 and n.d. (not detected)–12.82 µg/kg in apple and citrus peels, respectively. Morpholine was not detected in citrus or apple pulp samples or in vegetable samples.


1997 ◽  
Vol 80 (1) ◽  
pp. 63-73 ◽  
Author(s):  
Guo-Fang Pang ◽  
Yan-Zhong Cao ◽  
Chun-Lin Fan ◽  
Jin-Jie Zhang ◽  
Xue-Min Li

Abstract The stability of 8 synthetic pyrethroids in 9 crops during storage for 90 days were studied. The 8 pyrethroid insecticides were highly persistent in the 6 grains during storage. But their stabilities in 3 kinds of fruits and vegetables were different from those in the 6 grains: Most of them were degraded. Florisil purification conditions were studied with 6 batches of Florisil from 3 countries at various extents of deactivation and amounts. The best conditions of Florisil purification found in this present research agree with those found 1 year ago. The efficiencies of acetonitrile and acetone to extract the 8 pyrethroids from 6 fruit and vegetable samples were compared. The extraction efficiency of acetone was competitive with that of acetonitrile for the 6 fruit and vegetable samples. Method performance was evaluated by 6 analysts from different areas. The ruggedness tests demonstrate further that the proposed method is simple, accurate with good precision, and suitable for multiresidue analysis of pyrethroids in various agriculture products.


1979 ◽  
Vol 25 (11) ◽  
pp. 1944-1947 ◽  
Author(s):  
F J Frey ◽  
B M Frey ◽  
L Z Benet

Abstract The therapeutic response to and side effects of glucocorticoids will be better recognized and the recovery of the adrenals during the tapering of therapy with steroids better evaluated if endogenous and exogenous glucocorticoids are separately assessed. We describe a specific method for simultaneously measuring the concentrations of cortisone, cortisol, prednisone, and prednisolone in plasma by "high-pressure" liquid chromatography. The steroids, together with an internal standard, dexamethasone, are extracted from 1 mL of plasma with methylene chloride-ether, washed with acid and base, and separated isocratically on a normal-phase silica column with a mobile phase consisting of methylene chloride/tetrahydrofuran/methanol/glacial acetic acid (96.85/1/2.1/0.05 by vol) at a flow rate of 1.3 mL/min. The steroids are detected at 254 nm and quantitated by peak-height measurements; their retention times range from 6 to 20 min. The lower limits for routine detection of all four compounds is 10 microgram/L. The analytical recoveries are about 75%; the intra-day variability (CV) is 1 to 9%, and the inter-day variability 2 to 11%. Of 26 drugs and 20 steroids tested, only theophylline presents an interference problem.


1988 ◽  
Vol 71 (4) ◽  
pp. 748-760
Author(s):  
James L Daft

Abstract A gas chromatographic (GC) method is described for the determination of 22 fumigant and industrial chemical residues in a variety of foods. The fumigants and industrial chemicals determined are methyl bromide, methylene chloride, carbon disulfide, chloroform, 1,1-dichloroethane, ethylene dichloride, methyl chloroform, carbon tetrachloride, methylene bromide, propylene dichloride, 2,3-dichloropropene, trichloroethylene, 1,3-dichloropropylene, 1,1,2-trichloroethane, chloropicrin, ethylene dibromide, tetrachloroethylene, propylene dibromide, l,l,2,2-tetrachloroethane,j»-dichlorobenzene, o-dichlorobenzene, and l,2-dibromo-3-chloropropane. Except for the latter three, the fumigants are determined at 90°C on 3.6 m 20% loaded OV-101 columns with electron-capture and Hall-electroconductivity detectors. The other 3 compounds (o-dichlorobenzene, p-dichlorobenzene, and l,2-dibromo-3-chloropropane), which elute beyond 30 min on the above columns, are determined at 90°C on 1.8 m 5% loaded OV-101 columns with the same detectors. The ng/g-level fortifications have an overall mean analyte recovery of 70% and a coefficient of variation of 40%. The variety of foods examined includes both fatty and nonfatty food types (e.g., off-the-shelf cooked and uncooked grain-based items, dairy products, fresh and canned fruits and vegetables, and meats). Samples are extracted and cleaned up according to fat content and food type. Samples containing less than 71% fat are extracted by using an aqueous: nonaqueous shakeout (20% acetone solution under isooctane). Most extracts (isooctanes) are analyzed directly. Extracts from samples containing from 21 to 70% fat (e.g., ground beef, pecans, and corn chips) are cleaned up further on micro-Florisil columns to remove excess fat. A few other samples containing more than 71% fat or oil (e.g., butter, salad dressing, and vegetable oil) are diluted directly in isooctane and, depending on the degree of dilution, can be cleaned up further on micro-Florisil columns. Also, clear beverages (e.g., soda and tea) are extracted directly with isooctane. These extraction and cleanup techniques were tested on 231 different table-ready foods. Three-hundred incurred residues of 10 different fumigants were found in 138 items examined; 93 items had no detectable residues. The main advantage of the method is rapid semiquantitative determination of multiple fumigants from all food types.


2012 ◽  
Vol 554-556 ◽  
pp. 1459-1465
Author(s):  
Yun Hong Liu ◽  
Wen Xue Zhu ◽  
Lei Luo ◽  
Yu Song

Recently, vacuum far-infrared radiation (VFIR) drying has received more and more attention because of its effective and successful applications in drying agricultural products, fruits and vegetables. Drying characteristics of VFIR drying on Cornus officinalis was studied in this research, and orthogonal regression experiment was designed and carried out. The results showed that with increase of heater’s temperature and decrease of chamber’s pressure, drying rate and loganin content increase, and the influence of heater’s temperature is more significant than that of pressure. With nonlinear programming analysis method, the optimized process parameters are obtained as heater’s temperature 98.6 oC and pressure 1000 Pa, and the corresponding drying time and loganin content are 250 min and 1.18%, respectively.


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