Application of mixed solvents for elution of organophosphate pesticides extracted from raw propolis by matrix solid-phase dispersion and analysis by GC-MS

2014 ◽  
Vol 68 (11) ◽  
Author(s):  
Kati Medina-Dzul ◽  
David Muñoz-Rodríguez ◽  
Yolanda Moguel-Ordoñez ◽  
Cristian Carrera-Figueiras
Keyword(s):  
Solid Phase ◽  
Mixed Solvents ◽  
Solvent Mixture ◽  
Binary Solvent ◽  
Solvent Mixtures ◽  
Organophosphate Pesticides ◽  
Experimental Conditions ◽  
Matrix Solid Phase Dispersion ◽  
Phase Dispersion ◽  
Relative Standard

AbstractThe excessive application of organophosphate pesticides (OPPs) in crop fields close to hives and its application in beekeeping practices are potential sources of contamination of propolis. Pesticides were extracted from raw propolis by matrix solid-phase dispersion. Because of the complex chemical composition of propolis, binary solvent mixtures based on acetonitrile and a relatively non-polar solvent in different proportions were tested for the selective elution of OPPs. The effect of mixed solvents on clean-up was evaluated by GC-MS and the main interfering compounds co-eluted with pesticides were identified. In addition, three volumes of the solvent mixture and the volume of the sample were evaluated in an experimental factorial design. The final experimental conditions were 1 mL of dissolved propolis and 8 mL of acetonitrile/dichloromethane (g4 r = 25: 75). Mean recoveries ranged from 55 % to 96 % (relative standard deviation < 8 %) with an inter-day precision lower than 24 %. The proposed method was applied to the analysis of real samples obtained from local beekeepers.

scholarly journals Determination of Insecticides in Honey by Matrix Solid-Phase Dispersion and Gas Chromatography with Nitrogen–Phosphorus Detection and Mass Spectrometric Confirmation

2002 ◽  
Vol 85 (1) ◽  
pp. 128-133 ◽  
Author(s):  
Consuelo Sánchez-Brunete ◽  
Beatriz Albero ◽  
Ester Miguel ◽  
José Luis Tadeo
Keyword(s):  
Solid Phase ◽  
Single Step ◽  
Organophosphorus Insecticides ◽  
Matrix Solid Phase Dispersion ◽  
Phase Dispersion ◽  
Relative Standard ◽  
The Matrix ◽  
Low Volume ◽  
Nitrogen Phosphorus

Abstract A multiresidue method was developed for the determination of 12 organophosphorus insecticides (diazinon, parathion methyl, fenitrothion, pirimiphosmethyl, malathion, fenthion, chlorpyrifos, quinalphos, methidathion, ethion, azinphosmethyl, coumaphos), one carbamate (pirimicarb), and one amidine (amitraz) in unifloral and multifloral honeys. The analytical procedure was based on the matrix solid-phase dispersion of honey on a mixture of Florisil and anhydrous sodium sulfate in small glass columns and subsequent extraction with a low volume of hexane–ethyl acetate (90 + 10, v/v), assisted by sonication. The insecticide residues were determined by capillary chromatography with nitrogen–phosphorus detection and confirmed by mass spectrometry. Average recoveries at the 0.05–0.5 μg/g levels were &gt;80% for organophosphorus insecticides and about 60% for the other insecticides, pirimicarb and amitraz, with relative standard deviations &lt;10%. The detection limit for the different insecticides ranged between 6 and 15 μg/kg. The main advantages of the proposed method are that extraction and cleanup are performed in a single step with a low volume of organic solvent. The method is simple, rapid, and less laborious than conventional methods. Several Spanish honeys were analyzed with the proposed method and no residues of the studied insecticides were found.

scholarly journals Rapid MSPD-LC–MS/MS Procedure for Determination of Pesticides in Potato Tubers

2020 ◽  
Vol 58 (9) ◽  
pp. 831-843
Author(s):  
Magdalena Danek ◽  
Marcin Sajdak ◽  
Joanna Płonka ◽  
Hanna Barchańska
Keyword(s):  
Analytical Procedure ◽  
Solid Phase ◽  
Potato Tubers ◽  
Limit Of Quantification ◽  
Matrix Solid Phase Dispersion ◽  
Phase Dispersion ◽  
Relative Standard ◽  
Validation Parameters ◽  
Dispersion Technique

Abstract The program of potato protection recommended by the producers of agrochemicals requires application: thiamethoxam, lambda-cyhalothrin, deltamethrin, rimsulfuron and metalaxyl. Therefore, there is a risk that these pesticides are present in tubers, thus posing a toxicological risk to the consumer. In this respect, it is necessary to monitor the presence of these compounds in edible plants. Therefore, the aim of this paper was to develop a novel, simple and robust analytical procedure for simultaneous determination of above-mentioned pesticides in potato tubers. To develop an analytical procedure that fulfills SANTE demands, quick, easy, cheap, effective, rugged and safe method and matrix solid phase dispersion technique were investigated. The final determination was conducted by liquid chromatography with tandem mass spectrometry. The obtained experimental data were analyzed by analysis of variance. For the extraction of analytes, matrix solid phase dispersion with octadecyl sorbent and methanol as eluent was chosen, since it provides the validation parameters according to SANTE requirements (recovery: 77–111%, relative standard deviation: 1–10%, limit of quantification: 0.9–5.0 μg/kg). This innovative analytical procedure is a practical analytical tool, which was successfully proven by applying it for target pesticides determination in potato tuber samples of different varieties randomly chosen at local markets.

scholarly journals Effect of Pretreatment on Detection of 37 Pesticide Residues in Chrysanthemum indicum

2021 ◽  
Vol 2021 ◽  
pp. 1-12
Author(s):  
Xiao-Ying Lu ◽  
Yan-Qin Ouyang ◽  
Wei-Ya Zeng ◽  
Cui-Qing Lin ◽  
Lu-Hua Xiao ◽  
...  
Keyword(s):  
Matrix Effect ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Gas Chromatography Mass Spectrometry ◽  
Enhancement Effect ◽  
Matrix Solid Phase Dispersion ◽  
Phase Dispersion ◽  
Chrysanthemum Indicum ◽  
Relative Standard ◽  
Limit Of Quantitation

This study aimed to develop a method, followed by gas chromatography-mass spectrometry, for detecting 37 pesticides in Chrysanthemum indicum (C. indicum) and investigating the decrease in the matrix-induced enhancement effect. The influence of QuEChERS extraction and matrix solid-phase dispersion (MSPD) on the recovery and matrix effect (ME) was compared. extraction and matrix solid-phase dispersion (MSPD) on the recovery and matrix effect (ME) was compared to decrease the ME. The cleanup sorbents, volume and type of solvent, and treatment time were optimized. The accuracy (as recovery), precision (as relative standard deviation, RSD), linearity, limit of quantitation, and limit of detection were determined. The recoveries at the three levels using mixed standard solution ranged between 76% and 120% with RSD ≤15%, and 76% and 120% with RSD ≤11% for MSPD and QuEChERS extraction, respectively. The results suggested that the ME for 21 pesticides was in the range of 80%–120% after MSPD and 15% after QuEChERS extraction. QuEChERS extraction was simpler and faster than MSPD. This methodology was applied in the analysis of 27 C. indicum samples; phorate was most frequently detected (63.0% of the sample).

scholarly journals Stereo- and Enantioselective Determination of Pesticides in Soil by Using Achiral and Chiral Liquid Chromatography in Combination with Matrix Solid-Phase Dispersion

2003 ◽  
Vol 86 (3) ◽  
pp. 521-528 ◽  
Author(s):  
Zhao-Yang Li ◽  
Zhi-Chao Zhang ◽  
Qi-Lin Zhou ◽  
Qing-Min Wang ◽  
Ru-Yu Gao ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Stationary Phase ◽  
Chiral Stationary Phase ◽  
Solid Phase ◽  
Total Concentration ◽  
Environmental Media ◽  
Matrix Solid Phase Dispersion ◽  
Phase Dispersion ◽  
Relative Standard

Abstract The separation of enantiomers and diastereomers of 8 commonly used pesticides was investigated by liquid chromatography (LC) using a Chiralcel OD column (cellulose tris-3,5-dimethylphenyl-carbamate as the chiral stationary phase) and a Pirkle-type Chirex 3020 column (urea derivative from the reaction of (R)-1-(α-naphthyl)ethylamine with (S)-tert-leucine, chemically bonded to 3-aminopropylsilanized silica as the chiral stationary phase). The pesticides studied included one organophosphorus insecticide (phenthoate), 3 triazole fungicides (uniconazole, diniconazole, and propiconazole), and 4 pyrethroids (fenpropathrin, β-cypermethrin, β-cyfluthrin, and α-fenvalerate). The enantiomers were separated within 20 min with a resolution of ≥1.5 using a mixture of n-hexane and 2-propanol as the mobile phase for all the pesticides studied except propiconazole, for which only the 2 diastereomers were baseline separated. This method allows determination of the enantiomers or stereoisomers of the above pesticides in soil. The strategy was as follows: (1) First, the total concentration(s) of the enantiomer pair(s) of a chiral pesticide in soil was (were) determined by a newly developed matrix solid-phase dispersion (MSPD) procedure, followed by silica-based LC quantification. The recoveries ranged from 76.5 to 93.6% with relative standard deviations of 6.0%. (2) Second, the enantiomeric ratio(s) (ER(s)) of the chiral pesticide was (were) determined by LC with a chiral stationary phase after fractionation of the MSPD extract by silica-based LC. The determined ERs or stereoisomeric ratio(s) (SR(s); for propiconazole, only the SR of the 2 diastereomers was determined) in soil samples spiked with the above 8 racemic pesticides agreed with those of the corresponding standard solutions. (3) Third, based on the total concentrations and the corresponding ERs, the concentration of each enantiomer in soil was calculated. The proposed method is rapid, precise, and sensitive, and is appropriate for the investigation of the stereo- and enantioselective degradation of pesticides in environmental media.

scholarly journals Multiresidue Determination of Pesticides in Honey by Matrix Solid-Phase Dispersion and Gas Chromatography with Electron-Capture Detection

2001 ◽  
Vol 84 (4) ◽  
pp. 1165-1171 ◽  
Author(s):  
Beatriz Albero ◽  
Consuelo Sánchez-Brunete ◽  
José L Tadeo
Keyword(s):  
Gas Chromatography ◽  
Electron Capture ◽  
Solid Phase ◽  
Organophosphorus Compounds ◽  
Organophosphorus Pesticides ◽  
Electron Capture Detection ◽  
Matrix Solid Phase Dispersion ◽  
Phase Dispersion ◽  
Relative Standard

Abstract A multiresidue method was developed for the determination of 15 pesticides (organochlorines, organophosphorus compounds, pyrethroids, and other acaricides) in various commercial honeys (eucalyptus, lavender, orange, rosemary, and multifloral). The analytical procedure is based on the matrix solid-phase dispersion of honey in a mixture of Florisil and anhydrous sodium sulfate; the mixture is placed in small plastic columns and extracted with hexane–ethyl acetate (90 + 10, v/v). The pesticide residues are determined by capillary gas chromatography with electron-capture detection. Recoveries with the method at concentrations between 0.15 and 1.5 μg/g ranged from 80 to 113%, and relative standard deviations were &lt;10% for all the pesticides studied. The pesticide detection limits were within the range 0.5–5 mg/kg for organochlorines, around 3 μg/kg for the chlorinated organophosphorus pesticides studied, near 15 μg/kg for fluvalinate, and about 3 μg/kg for the other pyrethroids.

scholarly journals An Interlaboratory-Verified Method for the Determination of Vitamins Aand E inMilk- and Soy-Based Infant Formula by Liquid Chromatography with Matrix Solid-Phase Dispersion Extraction

2004 ◽  
Vol 87 (5) ◽  
pp. 1173-1178 ◽  
Author(s):  
G William Chase ◽  
Lin Ye ◽  
Vicky C Stoakes ◽  
Ronald R Eitenmiller ◽  
Austin R Long
Keyword(s):  
Infant Formula ◽  
Solid Phase ◽  
Extraction Procedure ◽  
Retinyl Palmitate ◽  
Tocopheryl Acetate ◽  
Matrix Solid Phase Dispersion ◽  
Phase Dispersion ◽  
Sample Extract ◽  
Relative Standard

Abstract An interlaboratory-verified, liquid chromatographic (LC) method is presented for determination of all-racemic α-tocopheryl acetate and retinyl palmitate in infant formula. The extraction procedure uses matrix solid-phase dispersion. A sample is mixed with C18, and the mixture is packed into a reservoir and eluted with selective solvents to extract the analytes. After evaporation and filtration, the sample extract is injected directly into a normal-phase LC system with fluorescence detection. All-racemic α-tocopheryl acetate and retinyl palmitate are quantitated isocratically with a mobile phase of hexane containing isopropanol at 0.2% (v/v) and 0.125% (v/v), respectively. A nonfortified zero control reference material (ZRM) was spiked at 5 levels, with 5 replicate analyses of 1/2x, x, 2x, 4x, and 16x where “x” represents the minimum levels of 250 IU/100 kcal (vitamin A) and 0.7 IU/100 kcal (vitamin E) as specified in Title 21 of the Code of Federal Regulations, part 107.100. Recoveries of retinyl palmitate ranged from 83.8 to 107%, and those of all-racemic α-tocopheryl acetate ranged from 87.7 to 108%. Two additional laboratories analyzed the ZRM samples at 4 spiking levels with 6 replicates. Recoveries of retinyl palmitate and all-racemic α-tocopheryl acetate ranged from 92.2 to 104% and from 91.7 to 101%, respectively, in the second laboratory. Recoveries of retinyl palmitate and all-racemic α-tocopheryl acetate ranged from 85.3 to 97.0% and from 86.6 to 110%, respectively, in the third laboratory. Relative standard deviations for all 3 laboratories ranged from 0.2 to 7.5% with an average of 2.9%. In addition, each laboratory analyzed a commercial milk- and commercial soy-based infant formula. Excellent agreement in results was obtained between the 3 laboratories for vitamins A and E in all matrixes.

scholarly journals DEVELOPMENT AND VALIDATION OF AN ANALYTICAL METHOD FOR THE DETERMINATION OF METHYLISOTHIAZOLINONE AND METHYLCHLOROISOTHIAZOLINONE IN COSMETIC PRODUCTS USING MATRIX SOLID-PHASE DISPERSION COUPLED TO GAS CHROMATOGRAPHY-MASS SPECTROMETRY

2021 ◽  
pp. 140-147
Author(s):  
NURINA PRAPURANDINA ◽  
HARMITA HARMITA ◽  
HERMAN SURYADI
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Analytical Method ◽  
Solid Phase ◽  
Cosmetic Products ◽  
Solid Sorbent ◽  
Matrix Solid Phase Dispersion ◽  
Phase Dispersion ◽  
Relative Standard ◽  
Limit Of Quantitation

Objective: This study was to develop the first simultaneous method for quantification of MI and MCI by using matrix solid-phase dispersion (MSPD) as an extraction technique followed by gas chromatography-tandem mass spectrometry (GC-MS) in cosmetic products to support that law enforcement. Methods: The MI and MCI were extracted from the cosmetic sample by using matrix solid-phase dispersion technique with alumina as solid sorbent and ethyl acetate as eluent. After being isolated, MI and MCI from the samples were analyzed using GC-MS equipped with DB-5MS capillary column. Results: The validated method for both leave-on and rinse-off cosmetic showed that MI and MCI recoveries were between 97.87-103.15 %, relative standard deviation (RSD) values were lower than 11%, and limit of quantitation (LOQ) values for the leave-on product were 0.96 µg/ml and 1.95 µg/ml and for rinse-off products were 0.56 µg/ml and 1.49 µg/ml for MI and MCI, respectively. Conclusion: This purposed analytical method for determining MI and MCI in cosmetic products using MSPD-GC-MS complies with the validation acceptance criteria.

scholarly journals Evaluation of Antibacterial Enrofloxacin in Eggs by Matrix Solid Phase Dispersion-Flow Injection Chemiluminescence

2014 ◽  
Vol 2014 ◽  
pp. 1-5 ◽  
Author(s):  
Xiaocui Duan ◽  
Pingping Zhang ◽  
Jing Feng ◽  
Ning Jiao
Keyword(s):  
Flow Injection ◽  
Solid Phase ◽  
Optimal Conditions ◽  
Testing Technique ◽  
Matrix Solid Phase Dispersion ◽  
Phase Dispersion ◽  
Relative Standard ◽  
Flow Injection Chemiluminescence ◽  
Simple Flow

The study based on the chemiluminescence (CL) reaction of potassium ferricyanide and luminol in sodium hydroxide medium, enrofloxacin (ENRO) could dramatically enhance CL intensities and incorporated with matrix solid-phase dispersion (MSPD) technique (Florisil used as dispersant, dichloromethane eluted the target compounds). A simple flow injection chemiluminescence (FL-CL) method with MSPD technique for determination of ENRO in eggs was described. Under optimal conditions, the CL intensities were linearly related to ENRO concentration ranging from4.0×10-8 g.L−1to5.0×10-5 g.L−1, with a correlation coefficient of 0.9989 and detection limit of5.0×10-9 g.L−1. The relative standard deviation was 3.6% at an ENRO concentration of2.0×10-6 g.L−1. Our testing technique can help ensure food safety, and thus, protect public health.

scholarly journals Development and Validation of a HPLC-UV Method for Simultaneous Determination of Five Sulfonylurea Herbicide Residues in Groundnut Oil Followed by Matrix Solid-Phase Dispersion

2012 ◽  
Vol 2012 ◽  
pp. 1-5 ◽  
Author(s):  
T. Nageswara Rao ◽  
A. Ramesh ◽  
T. Parvathamma
Keyword(s):  
Ethyl Acetate ◽  
High Performance ◽  
Solid Phase ◽  
Sulfonylurea Herbicide ◽  
Groundnut Oil ◽  
Herbicide Residues ◽  
Matrix Solid Phase Dispersion ◽  
Phase Dispersion ◽  
Relative Standard

A simple, sensitive, and inexpensive method was developed using matrix solid-phase dispersion (MSPD), together with high performance liquid chromatographic method for determination of sulfonylurea herbicide residues (nicosulfuron, pyrazosulfuron ethyl, metsulfuron methyl, chlorsulfuron and azimsulfuron) in groundnut oil. The evaluated parameters included the type and amount of sorbent (silica gel, C 18 and florisil) and the nature of eluent (ethyl acetate, dichloromethane, and acetonitrile). The best results were obtained using 1.0 g of groundnut oil sample, 1.0 g of C 18 as sorbent, and 20 mL of ethyl acetate-dichloromethane (1 : 1, (v/v)). The method was validated using groundnut oil samples spiked with sulfonylurea herbicides at different concentration levels (0.05 and 0.5 g/mL). Average recoveries (using each concentration six replicates) ranged 90–97%, with relative standard deviations less than 3%, the concentration of calibration solutions was in the range 0.01–2.0 g/mL and limits of detection (LOD) as well as limits of quantification (LOQ) were 0.01 g/mL and 0.05 g/mL, respectively.

scholarly journals Determination of Thiabendazole in Orange Juice and Rind by Liquid Chromatography with Fluorescence Detection and Confirmation by Gas Chromatography/Mass Spectrometry After Extraction by Matrix Solid-Phase Dispersion

2004 ◽  
Vol 87 (3) ◽  
pp. 664-670 ◽  
Author(s):  
Beatriz Albero ◽  
Consuelo Sánchez-Brunete ◽  
José L Tadeo
Keyword(s):  
Gas Chromatography ◽  
Liquid Chromatography ◽  
Fluorescence Detection ◽  
Orange Juice ◽  
Solid Phase ◽  
Extraction Column ◽  
Matrix Solid Phase Dispersion ◽  
Phase Dispersion ◽  
Relative Standard

Abstract A method was developed for the determination of thiabendazole (TBZ) in orange juice and rind based on matrix solid-phase dispersion (MSPD). TBZ was extracted with ethyl acetate and the extract was subsequently cleaned up on a solid-phase extraction column. Fungicide residues were determined by liquid chromatography with fluorescence detection. Recoveries through the method ranged from 87 to 97% with relative standard deviations ≤11%. The detection and quantitation limits were 0.15 and 0.50 μg/kg, respectively. The confirmation of TBZ residues in positive samples was performed by solid-phase microextraction followed by gas chromatography with mass spectrometric detection using selected ion monitoring. The developed method was applied to determine TBZ levels in commercial orange juices and in juice and rind of fresh oranges. The influence of storage and washing of fruits on TBZ residues was also studied.

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