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 Liquid Chromatographic Analysis of Vitamin K1 in Milk-Based Infant Formula with Matrix Solid-Phase Dispersion

1999 ◽  
Vol 82 (5) ◽  
pp. 1140-1145 ◽  
Author(s):  
G William Chase ◽  
Ronald R Eitenmiller ◽  
Austin R Long
Keyword(s):  
Infant Formula ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Reversed Phase ◽  
Vitamin K1 ◽  
Matrix Solid Phase Dispersion ◽  
Phase Dispersion ◽  
Limit Of Quantitation ◽  
Liquid Chromatographic Analysis ◽  
Liquid Chromatographic

Abstract A liquid chromatographic method for vitamin K1 in milk-based infant formula is described. The vitamins are extracted from infant formula by matrix solid-phase dispersion and quantitated by reversed-phase chromatography with fluorescence detection. Vitamin K1 is converted to the fluorescent hydroquinone with a postcolumn zinc reductive reactor. The limit of detection is 12 pg, and the limit of quantitation is 38 pg on-column. Linear responses were obtained in the range 0.55-22.1 ng/mL (r2 = 0.9998). Recoveries of vitamin K1 from an analyte-fortified blank material for milk-based infant formula averaged 91.7% (n = 25). The method provides a rapid, specific, and easily controlled assay for vitamin K1 in fortified infant formula.

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 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.

scholarly journals Processing of Flavor-Enhanced Oils: Optimization and Validation of Multiple Headspace Solid-Phase Microextraction-Arrow to Quantify Pyrazines in the Oils

Life ◽  
2021 ◽  
Vol 11 (5) ◽  
pp. 390
Author(s):  
Ziyan Xu ◽  
Chuan Zhou ◽  
Haiming Shi ◽  
Hong Zhang ◽  
Yanlan Bi ◽  
...  
Keyword(s):  
Solid Phase Microextraction ◽  
Incubation Temperature ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Gas Chromatography Mass Spectrometry ◽  
Extraction Temperature ◽  
Headspace Solid Phase Microextraction ◽  
Flavor Analysis ◽  
Relative Standard ◽  
Limit Of Quantitation

An efficient and effective multiple headspace-solid phase microextraction-arrow-gas chromatography-mass spectrometry (MHS-SPME-arrow-GCMS) analytical protocol is established and used to quantify the flavor compounds in oils. SPME conditions, such as fiber coating, pre-incubation temperature, extraction temperature, and time were studied. The feasibility was compared between SPME-arrow and the traditional fiber by loading different sample amounts. It was found that the SPME-arrow was more suitable for the MHS-SPME. The limit of detection (LODs) and limit of quantitation (LOQs) of pyrazines were in the range of 2–60 ng and 6–180 ng/g oil, respectively. The relative standard deviation (RSD) of both intra- and inter-day were lower than 16%. The mean recoveries for spiked pyrazines in rapeseed oil were in the range of 91.6–109.2%. Furthermore, this newly established method of MHS-SPME-arrow was compared with stable isotopes dilution analysis (SIDA) by using [2H6]-2-methyl-pyrazine. The results are comparable and indicate this method can be used for edible oil flavor analysis.

scholarly journals Determination of Polycyclic Aromatic Hydrocarbons in Honey by Matrix Solid-Phase Dispersion and Gas Chromatography/Mass Spectrometry

2003 ◽  
Vol 86 (3) ◽  
pp. 576-582 ◽  
Author(s):  
Beatriz Albero ◽  
Consuelo Sánchez-Brunete ◽  
José L Tadeo
Keyword(s):  
Gas Chromatography ◽  
Polycyclic Aromatic Hydrocarbons ◽  
Aromatic Hydrocarbons ◽  
Solid Phase ◽  
Gas Chromatography Mass Spectrometry ◽  
Matrix Solid Phase Dispersion ◽  
Phase Dispersion ◽  
Relative Standard ◽  
Polycyclic Aromatic

Abstract A multiresidue method was developed for the determination of 16 polycyclic aromatic hydrocarbons (PAHs) in unifloral and multifloral honeys. The analytical procedure is based on the matrix solid-phase dispersion of honey on a mixture of Florisil and anhydrous sodium sulfate in small glass columns and extraction with hexane–ethyl acetate (90 + 10, v/v) with assisted sonication. The PAH residues are determined by gas chromatography with mass spectrometric detection using selected-ion monitoring. Average recoveries for all the PAHs studied were in the range of almost 80 to 101%, with relative standard deviations of 6 to 15%. The limits of detection ranged from 0.04 to 2.9 μg/kg. The simultaneous extraction and cleanup of samples makes this method simple and rapid, with low consumption of organic solvents.

scholarly journals Accelerated Solvent Extraction of Vitamin K1 in Medical Foods in Conjunction with Matrix Solid-Phase Dispersion

2000 ◽  
Vol 83 (2) ◽  
pp. 407-410 ◽  
Author(s):  
G William Chase ◽  
Brian Thompson
Keyword(s):  
Solvent Extraction ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Reversed Phase ◽  
Accelerated Solvent Extraction ◽  
Vitamin K1 ◽  
Matrix Solid Phase Dispersion ◽  
Phase Dispersion ◽  
Limit Of Quantitation ◽  
Medical Foods

Abstract An extraction technique is described for vitamin K1 in medical foods, using accelerated solvent extraction (ASE) in conjunction with matrix solid-phase dispersion (MSPD). The medical food sample is treated as it would be with MSPD extraction, followed by ASE for a hands-free automated extraction. The vitamin K1 in the ASE extract is then quantitated by reversed-phase liquid chromatography with fluorescence detection. The chromatography specifications are identical to those in previous work that used MSPD only, with a limit of detection of 6.6 pg and a limit of quantitation of 22 pg on column. Recoveries, which were determined for an analyte-fortified zero control reference material for medical foods, averaged 97.6% (n = 25) for vitamin K1. The method provides a rapid, automatic, specific, and easily controlled assay for vitamin K1 in fortified medical foods with minimal solvent usage.

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.

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