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.

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.

Simultaneous Determination of Four Herbicide and Pesticide Residues in Chinese Green Tea Using QuEChERS Purification Procedure and UPLC-MS/MS Analysis

2013 ◽  
Vol 634-638 ◽  
pp. 1586-1590
Author(s):  
Su Fang Wang ◽  
Shou Jie Zhang ◽  
Chun Hong Dong ◽  
Guo Qing Wang ◽  
Jun Feng Guo ◽  
...  
Keyword(s):  
Formic Acid ◽  
Simultaneous Determination ◽  
Green Tea ◽  
Limit Of Detection ◽  
Multiple Reaction Monitoring ◽  
Graphitized Carbon Black ◽  
Ms Analysis ◽  
Relative Standard ◽  
Limit Of Quantitation

A method for simultaneous determination of residuals of four herbicides and pesticides, simazine, carboxin, diflubenzuron and rotenone, in Chinese green tea was developed. In the proposed method, the tea powder was placed in a centrifuge tube with a plug, extracted in saturated aqueous sodium chloride solution and acetonitrile, agitated using vortex oscillator, and then centrifuged 5 min at 4000 rpm. The supernatant solution was purified by primary secondary amine (PSA) sorbent, C18 power, and graphitized carbon black powder, respectively. Then the purified extracts were dissolved with acetonitrile:0.1% formic acid aqueous solution (40:60, V/V) and agitated, filtered using a syringe with 0.22 μm nylon filter prior to UPLC-MS/MS analysis. The UPLC analysis was performed on an ACQUITY UPLC® HSS T3 column (2.1 mm×100 mm, 1.8 µm), using acetonitrile-0.1% formic acid as mobile phase with the flow rate as 0.3 mL•min-1. Injection volume was 10 µL. Positive ionization mode was applied, and the ions were monitored in the multiple reaction monitoring (MRM) mode with curtain gas 0.069 MPa, collision gas 0.052 MPa, ESI ion spray voltage 5000 V, temperature 550 °C, nebulizer gas 0.24 MPa, and turbo gas 0.28 MPa. The limit of detection (LOD) and limit of quantitation (LOQ) of the proposed method are 1 μg•kg-1and 5 μg•kg-1, respectively. The average recoveries of the four pesticides at 10, 20, and 50 µg•kg-1spiking levels range from 77.4% to 95.3%. TheSupersSuperscript textcript textrelative standard deviation (RSD) (n=6) range form 11.83% to 4.52%.

scholarly journals Development and validation of a rapid selective high-throughput LC-MS/MS method for the determination of triclabendazole sulfoxide concentrations in sheep plasma and its use in bioequivalence studies

2021 ◽  
Author(s):  
Lénárd Farczádi ◽  
Álmos Dósa ◽  
Orsolya Melles ◽  
Laurian Vlase
Keyword(s):  
Formic Acid ◽  
Flow Rate ◽  
Mobile Phase ◽  
Liver Fluke ◽  
Internal Standard ◽  
Gradient Elution ◽  
Sample Processing ◽  
Development And Validation ◽  
Analytical Separation

AbstractTriclabendazole is one of the main drugs used to treat liver fluke in livestock. A rapid LC-MS/MS method was developed and validated to determine ovine plasma levels of triclabendazole sulfoxide.A Gemini NX-C18 column was used to achieve analytical separation, with gradient elution of a mobile phase composed of 0.1% formic acid in acetonitril and 0.1% formic acid in water at flow rate of 0.6 mL/min. MRM with positive ESI ionization was used for the detection of triclabendazole sulfoxide (m/z 360.10 from m/z 376.97). Fenbendazole was used as internal standard. Plasma protein precipitation with acetonitrile was used for sample processing.The method was validated with regards to selectivity, linearity (r > 0.9939), within run and between run precision (CV < 8.9%) and accuracy (bias < 8.9%) over the concentration range 1–100 µg/mL plasma.The method developed is simple, selective and can be applied in bioequivalence and bioavailability studies.

scholarly journals Development of a UHPLC-MS/MS method for the determination of quercetin in milk and its application to a pharmacokinetic study

2019 ◽  
Vol 63 (1) ◽  
pp. 87-91
Author(s):  
Małgorzata Gbylik-Sikorska ◽  
Anna Gajda ◽  
Artur Burmańczuk ◽  
Tomasz Grabowski ◽  
Andrzej Posyniak
Keyword(s):  
Formic Acid ◽  
Mobile Phase ◽  
High Performance ◽  
Therapeutic Agent ◽  
Clinical Mastitis ◽  
Liquid Extraction ◽  
Liquid Liquid Extraction ◽  
Repeatability And Reproducibility ◽  
The Mean

Abstract Introduction: Quercetin is a polyphenolic flavonoid which has been used in traditional Chinese medicine as a natural therapeutic agent with a broad spectrum of activities (antioxidant, anticancer, neuroprotective, anti-inflammatory, antiviral and antibacterial). The aim of this study was to develop and validate a rapid and simple ultra-high-performance liquid chromatography with tandem mass spectrometry (UHPLC-MS/MS) method for the determination of quercetin in milk. Material and Methods: Sample preparation was based on a liquid-liquid extraction with 0.5% formic acid in acetonitrile. The chromatographic separation was performed on a ZORBAX SB-C18 column with methanol and 0.5% formic acid as a mobile phase. Results: The procedure was successfully validated. The mean recovery of the analyte was 98%, with the corresponding intra- and inter-day variation less than 10% and 15%, respectively, and the repeatability and reproducibility were in the range of 3%–7.2% and 6.1%–12%, respectively. The lowest level of quantification was 1.0 μg/kg. Conclusion: The proposed method was successfully applied in evaluating the pharmacokinetics of quercetin in milk obtained from dairy cows with clinical mastitis after intramammary administration.

scholarly journals Development and Validation of Gas Chromatography-Triple Quadrupole Mass Spectrometric Method for Quantitative Determination of Regulated Plasticizers in Medical Infusion Sets

2018 ◽  
Vol 2018 ◽  
pp. 1-9 ◽  
Author(s):  
So Hyeon Jeon ◽  
Yong Pyo Kim ◽  
Younglim Kho ◽  
Jeoung Hwa Shin ◽  
Won Hyun Ji ◽  
...  
Keyword(s):  
Gas Chromatography ◽  
Quantitative Determination ◽  
Multiple Reaction Monitoring ◽  
Spectrometric Method ◽  
Mass Spectrometric Method ◽  
Triple Quadrupole ◽  
Quadrupole Mass ◽  
Ms Analysis ◽  
Relative Standard

A method for the quantitative determination of dibutyl phthalate (DBP), benzyl butyl phthalate (BBP), bis(2-ethylhexyl) adipate (DEHA), bis(2-ethylhexyl) phthalate (DEHP), di-n-octyl phthalate (DNOP), dioctyl terephthalate (DOTP), diisononyl phthalate (DINP), and diisodecyl phthalate (DIDP) in medical infusion sets was developed and validated using gas chromatography coupled with triple quadrupole mass spectrometry (GC-MS/MS) in the multiple reaction monitoring (MRM) mode. Solvent extraction with polymer dissolution for sample preparation was employed prior to GC-MS/MS analysis. Average recoveries of the eight target analytes are typically in the range of 91.8–122% with the relative standard deviations of 1.8–17.8%. The limits of quantification (LOQs) of the analytical method were in the ranges of 54.1 to 76.3 ng/g. Analysis using GC-MS/MS provided reliable performance, as well as higher sensitivity and selectivity than GC-MS analysis, especially for the presence of minority plasticizers at different concentrations.

Single-Laboratory Validation of a Method for the Determination of Vitamin D3 in Dietary Supplements by Liquid Chromatography with Tandem Mass Spectrometry (LC-MS/MS)

2014 ◽  
Vol 97 (2) ◽  
pp. 403-408
Author(s):  
Victor K M Lam ◽  
Ray C T Hung ◽  
Ella L M Wong ◽  
Johnny Y W Fok ◽  
Yiu-Chung Wong
Keyword(s):  
Formic Acid ◽  
Dietary Supplements ◽  
Vitamin D3 ◽  
Time Window ◽  
Collaborative Study ◽  
Internal Standard ◽  
Ammonium Formate ◽  
Soft Gels ◽  
Single Laboratory

Abstract A single-laboratory validation (SLV) for the analysis of vitamin D3 was performed in four types of dietary supplements (capsules, soft gels, syrups, and tablets) using LC-MS/MS. Samples were treated by alkaline saponification for oil-based soft gels and utilized EDTA solution for capsules, syrups,and tablets prior to n-hexane extraction. Vitamin D3 in sample extracts was separated on a reversed-phase C18 column (100 × 2.1 mm, 2.7 μm) using a mobile phase of a 95 + 5 (v/v) mixture of 5 mM ammonium formate in methanol containing 0.1% formic acid and 5 mM ammonium formate in 0.1% formic acid running at a flow rate of 0.2 mL/min. Vitamin D3 was confirmed by the presence of three fragment ions at m/z 107, 159, and 259 within a defined retention time window from the precursor ion at m/z 385. Quantitation was based on the peak area at m/z 367 to that of the internal standard (d3-vitamin D3) at m/z 370 with reference to the respective response ratios of the calibration standards. The linear response of vitamin D3 ranged from 0.10 to 6.29 mg/L and the correlation coefficient (r) of the six-point calibrationcurves was &gt;0.999. Accuracy, in terms of the spiked recoveries from blank syrup and starch powder at three different concentration levels, was 101–103%. Precision, determined by two different analysts over a period of 5 weeks, ranged from 2.7 to 7.0%for the four preparations. The SLV demonstrates the present LC-MS/MS method is reliable and robust for the determination of vitamin D3 in the studied dietary supplements. Considering the attainmentof satisfactory SLV results, further validation through intra-laboratory collaborative study is recommended.

scholarly journals Development and Validation of a Stability Indicating LC Method for the Assay and Related Substances Determination of a Proteasome Inhibitor Bortezomib

2012 ◽  
Vol 2012 ◽  
pp. 1-13 ◽  
Author(s):  
Kasa Srinivasulu ◽  
Mopidevi Narasimha Naidu ◽  
Kadaboina Rajasekhar ◽  
Murki Veerender ◽  
Mulukutla Venkata Suryanarayana
Keyword(s):  
Formic Acid ◽  
Mobile Phase ◽  
Gradient Elution ◽  
Hplc Method ◽  
Forced Degradation ◽  
Balance Study ◽  
Stability Indicating ◽  
Related Substances ◽  
Mass Balance Study

A novel, simple, sensitive, stability indicating HPLC method was developed and validated for quantification of impurities (process related and degradants) and assay determination of bortezomib. Stability indicating power of the method was established by forced degradation experiments and mass balance study. The chromatographic separation was achieved with Waters SymmetryShield RP18 column using gradient elution using the mobile phase-A consists of a mixture of water-acetonitrile-formic acid (715 : 285 : 1, v/v/v) and the mobile phase-B consists a mixture of methanol-water-formic acid (800 : 200 : 1, v/v/v), respectively. The developed method is validated for parameters like precision, accuracy, linearity, LOD, LOQ, and ruggedness. Central composite experimental design (CCD) was applied to check the robustness of the method. The stability tests were also performed on drug substances as per ICH norms.

Stability of cyclopiazonic acid in solution

2010 ◽  
Vol 3 (1) ◽  
pp. 25-33 ◽  
Author(s):  
G. Diaz ◽  
W. Thompson ◽  
P. Martos
Keyword(s):  
Mass Spectrometry ◽  
Formic Acid ◽  
Mobile Phase ◽  
Cyclopiazonic Acid ◽  
Tandem Mass ◽  
Considerable Difficulty ◽  
Ambient Oxygen ◽  
Carry Over ◽  
Chromatographic Parameters

Cyclopiazonic acid (CPA) is an important mycotoxin given its toxicity and prevalence in foods and feeds. There is tremendous interest in developing analytical methods that include CPA as part of a multi-residue mycotoxin routine, but there appears to be considerable difficulty in analysing it using liquid chromatography with electrospray ionisation tandem mass spectrometry (LC-MS/MS). During the development of a multi-residue method for mycotoxins including CPA, a number of issues were discovered under routine and common analytical conditions that have an impact on the determination of CPA, including: (1) at the ng/ml level CPA reacts with ambient oxygen from the headspace of the vial, an effect that decreases its concentration linearly; (2) CPA readily adsorbs to plastic in a reversible fashion; (3) CPA is acid hydrolysed with formic acid; (4) CPA reacts with the column stationary phase affecting chromatographic parameters; and (5) CPA presents significant carry-over issues. In an effort to find solutions to these problems we found that CPA can be protected from reacting with oxygen by adding 1 µg/ml ascorbic acid and that its carry-over can be reduced to a negligible level by injecting ammonia between injections of solutions containing CPA, even with formic acid in the mobile phase. Chromatographic conditions for CPA have been optimised in consideration of all of the aforementioned concerns.

Sign in / Sign up

Export Citation Format

Share Document