A Modified QuEChERS Extraction and LC-MS/MS Method for the Determination of Pesticide Residues in Curry Leaves (Murraya koenigii)

2019 ◽  
Vol 6 (1) ◽  
pp. 30-41
Author(s):  
Ranjith Arimboor ◽  
Karunkara Ramakrishna Menon ◽  
Natarajan Ramesh Babu ◽  
Haneesh Chandran
Keyword(s):  
Sample Preparation ◽  
Matrix Effect ◽  
Retention Time ◽  
Pesticide Residues ◽  
Mobile Phase ◽  
Preparation Technique ◽  
Modified Quechers ◽  
Curry Leaves ◽  
Ms Analysis ◽  
The Matrix

Background:Increased consumer demand for curry leaves free from pesticides demands fast and reliable analytical methods for the analysis of pesticide residues.Objective:The optimization of a QuEChERS based sample preparation technique with improved analytical accuracy by removing interfering matrix components for LC-MS/MS analysis of pesticide residues from curry leaves.Methods:A modified QuEChERS solid phase extraction method was developed and validated for the analysis of 26 pesticides in fresh and dried curry leaves. The effects of the sample preparation steps and column retention time on the matrix suppression of analyte ions were also evaluated.Results:Validation parameters were found within an acceptable range. The matrix effect evaluation studies showed that the QuEChERS sample preparation was able to minimize the ion suppression of analytes due to co-eluting matrix of components and that a d-SPE clean up step had major role in reducing matrix effect. The gradient mobile phase with longer retention time for analytes resulted in comparatively lesser matrix effects than the isocratic mobile phase of non-polar nature. Even after the clean up, a considerable number of compounds had more than 20% reduction in their MS response in the gradient mobile phase.Conclusion:This study emphasized the need of proper sample clean up before a LC-MS/MS analysis and the usage of matrix matched standards and mobile phase that ultimately results in an appropriate analyte separation in reasonable retention times.

scholarly journals Screening of multiclass pesticide residues in maca and Moringa oleifera by a modified QuEChERS sample preparation procedure and UPLC-ESI-MS/MS analysis

RSC Advances ◽  
2020 ◽  
Vol 10 (60) ◽  
pp. 36906-36919
Author(s):  
Yanqin Zhu ◽  
Ping Du ◽  
Jun Yang ◽  
Qinhong Yin ◽  
Yaling Yang
Keyword(s):  
Sample Preparation ◽  
Pesticide Residues ◽  
Moringa Oleifera ◽  
Simultaneous Analysis ◽  
Preparation Procedure ◽  
Safe Method ◽  
Esi Ms ◽  
Modified Quechers ◽  
Ms Analysis ◽  
Sample Preparation Procedure

In the present study, a modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) method was proposed for the simultaneous analysis of 75 pesticides in maca and Moringa oleifera with UPLC-ESI-MS/MS.

Determination of Nine Fungicides in Grape and Wine Using QuEChERS Extraction and LC/MS/MS Analysis

2015 ◽  
Vol 98 (6) ◽  
pp. 1745-1751 ◽  
Author(s):  
Gracia Martínez ◽  
Ascensión Morales ◽  
Alba Maestro ◽  
Sandra Cermeño ◽  
José Oliva ◽  
...  
Keyword(s):  
Formic Acid ◽  
Mobile Phase ◽  
Ammonium Formate ◽  
Safe Procedure ◽  
Triple Quadrupole ◽  
Acceptance Criteria ◽  
Analytic Procedure ◽  
Modified Quechers ◽  
Ms Analysis

Abstract An analytic procedure was developed for the determination of the fungicides ametoctradin, boscalid, cyazofamid, dimethomorph, fenhexamid, kresoxim–methyl, mepanipyrim, metrafenone, and pyraclostrobin in grape and wine. A modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) procedure was used for the extraction. Analysis of the extract was performed by LC/triple quadrupole-MS/MS. A Poroshell 120 EC-C18 column was used with a programmed gradient mobile phase consisting of (A) acetonitrile containing 0.1% formic acid and (B) water containing 0.1% formic acid and 2 mM ammonium formate. The acceptance criteria for the method were those proposed in the SANCO guide. The method was linear for the range of concentration studied (5–100 μg/L), and R2 values were higher than 0.998 and RSD values below 18%. Recovery was over 73.2% in grape and 76.7% in wines, and there was no case of more than 100% recovery. The recovery RSDs in reproducibility conditions were below 17.13% in grape and 15.6% in wines.

scholarly journals Determination of Pesticide Residues by GC-MS Using Analyte Protectants to Counteract the Matrix Effect

2005 ◽  
Vol 21 (11) ◽  
pp. 1291-1296 ◽  
Author(s):  
Consuelo SÁNCHEZ-BRUNETE ◽  
Beatriz ALBERO ◽  
Germán MARTÍN ◽  
José L. TADEO
Keyword(s):  
Matrix Effect ◽  
Pesticide Residues ◽  
The Matrix ◽  
Analyte Protectants

scholarly journals Accurate Determination, Matrix Effect Estimation, and Uncertainty Evaluation of Three Sulfonamides in Milk by Isotope Dilution Liquid Chromatography-Tandem Mass Spectrometry

2021 ◽  
Vol 2021 ◽  
pp. 1-7
Author(s):  
Chaonan Han ◽  
Xiuqin Li ◽  
Hui Jiao ◽  
Yan Gao ◽  
Qinghe Zhang
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Matrix Effect ◽  
Mobile Phase ◽  
Accurate Determination ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass

Liquid chromatography-tandem mass spectrometry (LC-MS/MS) is the most commonly used method for sulfonamide determination. Its accuracy, however, can be affected by many factors. In this study, sulfadiazine (SDZ), sulfadimidine (SMZ), and sulfadimethoxine (SDM) in milk were selected to investigate an accurate determination method and the potential influencing factors in the use of ultrahigh-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). Milk samples were extracted by 25 mL perchloric acid solution (pH = 2) and cleaned up using HLB solid-phase extraction (SPE) cartridges. Four kinds of filters, including PTFE, GHP, nylon, and glass fiber, were compared, and PTFE was selected since it had the best recoveries of target sulfonamides (SAs). Three quantitative methods, including external standard (ES), matrix matching (MM), and isotope dilution mass spectrometry (IDMS), were compared, among which IDMS exhibited the best accuracy. The matrix effect under different mobile phase compositions and of different sample matrices were evaluated and discussed. Ion suppression effects were observed during the determination of all SAs, which got stronger with the increase of the methanol composition percent in the mobile phase. After correction by IDMS, the matrix effect could be neglected. Matrix spiked recoveries at three spiked levels (1 μg/kg, 10 μg/kg, and 20 μg/kg) ranged from 96.8% to 103.8% by IDMS. The expanded relative uncertainties were in the range of 2.02% to 5.75%. The method exhibited wide application range, high accuracy, good stability, and high sensitivity.

scholarly journals Electrospray Ionization Matrix Effect as an Uncertainty Source in HPLC/ESI-MS Pesticide Residue Analysis

2010 ◽  
Vol 93 (1) ◽  
pp. 306-314 ◽  
Author(s):  
Anneli Kruve ◽  
Koit Herodes ◽  
Ivo Leito
Keyword(s):  
Electrospray Ionization ◽  
Matrix Effect ◽  
Matrix Effects ◽  
Residue Analysis ◽  
Commodity Group ◽  
Large Variability ◽  
Esi Ms ◽  
Ms Analysis ◽  
The Matrix ◽  
Peak Areas

Abstract The matrix effects in HPLC/electrospray ionization (ESI)-MS analysis are difficult to compensate for because of their large variability. It is, therefore, often more practical to include uncertainty due to the matrix effect into the uncertainty budget rather than try to compensate. This work presents an empirical approachthe matrix effect graph approachfor estimating the uncertainty due to the matrix effect in HPLC/ESI-MS analysis of pesticide residues in fruits and vegetables. At certain time intervals (1 month), a calibration graph using extracts of different fruits/vegetables as calibration solutions is prepared, and a regression line is fitted through these data. These fruits/vegetables may be either from the commodity group of the samples or from different commodity groups. The relative residuals of the calibration point peak areas are calculated and plotted against the measurement time. We term the resulting graph the matrix effect graph. The root mean square of the relative residuals is calculated and used as the estimate of relative uncertainty of the sample peak areas caused by the matrix effect. The matrix effect graph obtained over fruits/vegetables from different commodity groups can also be used to identify fruits/vegetables with extreme matrix effects. The matrix effect graph approach was used for determination of thiabendazole, aldicarb, imazalil, and methiocarb and was validated with tomato, cucumber, and sweet corn matrixes at the 0.5 mg/kg concentration level. When different commodity groups were used to compile the matrix effect graph, results of analysis of all samples agreed with the spiked concentrations within the expanded uncertainties (at k = 2 level). When the matrix effect graph was compiled using fruits from the same commodity group as the analyzed samples (fruiting vegetables in this case), agreement was found in 98 of the cases.

Comparison of Different Sample Preparation Techniques for Untargeted Metabolomics utilizing Q-TOF LC/MS and MetaboAnalyst 4.0

2020 ◽  
Vol 08 ◽  
Author(s):  
Ozan Kaplan ◽  
Engin Koçak ◽  
Mustafa Çelebier
Keyword(s):  
Sample Preparation ◽  
Solid Phase Extraction ◽  
Solid Phase ◽  
Phase Extraction ◽  
Preparation Technique ◽  
Sample Preparation Technique ◽  
Ms Analysis ◽  
Ionization Mode ◽  
Human Blood Samples ◽  
Preparation Techniques

Background: Profiling the whole metabolome with a single injection is not an easy process because the chemical and physical properties of metabolites are totally different within each other and the analytical methodologies and datamining procedures need lots of effort to make such an approach for real. This reality leads researchers to select an already applied methodology for metabolite profiling and analyze the samples through identical techniques. Objective: In this study, it was focused whether the sample preparation techniques on human blood samples prior to QTOF LC/MS analysis affect the number of detectable peaks and to analyze the matched metabolites of these peaks. The results were compared within each other. Method: Precipitation of proteins with methanol, ultrafiltration (Amicon® Ultra 3 kDa 0.5 mL Centrifugal Filters), liquidphase extraction (EXtrelut® NT 3 cartridges) and solid-phase extraction (Supelco HybridSPE®-Phospholipid Cartridge) were used for sample preparation on commercial pooled plasmas samples. C18 column (Agilent Zorbax 1.8 μM, 50 x 2.1 mm) was used as the chromatography column. Q-TOF LC/MS analysis was performed on positive ionization mode. XCMS and MetaboAnalyst 4.0 - MS Peaks to Pathways utility were used to evaluate the raw data. Results: Although the number of detected peaks through precipitation with methanol was the highest one (624 peaks), the detected peaks observed through ultrafiltration sample preparation technique matched with the highest number of metabolite peaks (151 metabolites). The number of the matched peaks with metabolites on liquid phase extraction (81 metabolites) was higher than the ones for solid phase extraction (29 metabolites). Conclusion: The results in this study may provide a novel perspective to analytical chemists working with clinicians to select their sample preparation technique prior to Q-TOF LC/MS based untargeted metabolomic approaches.

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