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 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 >80% for organophosphorus insecticides and about 60% for the other insecticides, pirimicarb and amitraz, with relative standard deviations <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.

Matrix solid-phase dispersion technique for the determination of moxidectin in bovine tissues

The Analyst ◽  
1996 ◽  
Vol 121 (10) ◽  
pp. 1469 ◽  
Author(s):  
M. Alvinerie ◽  
J. F. Sutra ◽  
D. Capela ◽  
P. Galtier ◽  
A. Fernandez-Suarez ◽  
...  
Keyword(s):  
Solid Phase ◽  
Matrix Solid Phase Dispersion ◽  
Phase Dispersion ◽  
Dispersion Technique

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 <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 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.

scholarly journals Determination of Six Pesticides in the Medicinal Herb Cordia salicifolia by Matrix Solid-Phase Dispersion and Gas Chromatography/Mass Spectrometry

2009 ◽  
Vol 92 (4) ◽  
pp. 1184-1189 ◽  
Author(s):  
Pedro Henrique Viana De Carvalho ◽  
Vanessa De Menezes Prata ◽  
Pricles Barreto Alves ◽  
Sandro Navickiene
Keyword(s):  
Extraction Method ◽  
Solid Phase ◽  
Gas Chromatography Mass Spectrometry ◽  
Neutral Alumina ◽  
Appetite Suppressant ◽  
Matrix Solid Phase Dispersion ◽  
Phase Dispersion ◽  
Relative Standard ◽  
Concentration Levels

Abstract A simple and effective extraction method based on matrix solid-phase dispersion was developed for acephate, chlorpropham, pyrimicarb, bifenthrin, tetradifon, and phosalone in leaves of the medicinal plant Cordia salicifolia, whose extracts are commercialized in Brazil as diuretic, appetite suppressant, and weight loss products. The determination method was GC/MS with selectedion monitoring. Different parameters of the method were evaluated, such as type of solid phase (C18, alumina, silica gel, and Florisil) and the amount of solid phase and eluent (dichloromethane, ethyl acetate, chloroform, and cyclohexane). The best results were obtained using 0.5 g herb sample, 0.5 g neutral alumina as the dispersant sorbent, 0.5 g C18 as the cleanup sorbent, and cyclohexanedichloromethane (3 + 1, v/v) as the eluting solvent. The method was validated using herb samples fortified with pesticides at different concentration levels (0.3, 0.5, and 1.0 mg/kg). Average recoveries (seven replicates) ranged from 67.7 to 129.9, with relative standard deviations between 6.3 and 26. Detection and quantitation limits for the herb ranged from 0.10 to 0.15 and 0.15 to 0.25 mg/kg, respectively.

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