Comparison of SPE/d-SPE and QuEChERS-Based Extraction Procedures in Terms of Fungicide Residue Analysis in Wine Samples by HPLC–DAD and LC-QqQ-MS

2016 ◽  
Vol 99 (6) ◽  
pp. 1436-1443 ◽  
Author(s):  
Tomasz Tuzimski ◽  
Tomasz Rejczak ◽  
Dominika Pieniążek ◽  
Grzegorz Buszewicz ◽  
Grzegorz Teresiński
Keyword(s):  
Multiple Reaction Monitoring ◽  
Residue Analysis ◽  
High Sensitivity ◽  
Extraction Procedures ◽  
Multiple Reaction Monitoring Mode ◽  
Sensitivity And Selectivity ◽  
Dispersive Spe ◽  
Array Detection ◽  
Fungicide Residue

Abstract Two different extraction and clean-up protocols, based on either the SPE/dispersive SPE (d-SPE) or the quick, easy, cheap, effective, rugged, and safe approach, were optimized and compared for determination of six selected fungicides (benalaxyl, metalaxyl, triadimenol, tebuconazole, diniconazole, and epoxiconazole) in wine samples. The pilot study was performed by applying HPLC with diode-array detection, and optimized procedures were easily transferred to the LC triple-quadrupole MS system. Both extraction procedures presented good performance for all the analytes, with recoveries in the range of 70–132% and SDs ≤20%. The d-SPE clean-up step included in both procedures allows obtaining colorless extracts with the majority of coextracted matrix compounds removed. LC with electrospray ionization and tandem MS operating in the multiple reaction monitoring mode provide high sensitivity and selectivity for trace analysis. Both developed procedures were evaluated in terms of commercial wine sample analysis. In three wine samples, metalaxyl and tebuconazole residues were detected at concentrations from 0.14 to 30.7 ng/mL. Both approaches showed satisfactory feasibility for fungicide residue analysis in wine samples.

QuEChERS-Based Extraction Procedures for the Analysis of Bisphenols S and A in Breast Milk Samples by LC-QqQ-MS

2019 ◽  
Vol 102 (1) ◽  
pp. 23-32 ◽  
Author(s):  
Tomasz Tuzimski ◽  
Dominika Pieniążek ◽  
Grzegorz Buszewicz ◽  
Grzegorz Teresiński
Keyword(s):  
Breast Milk ◽  
Solid Phase ◽  
Multiple Reaction Monitoring ◽  
High Sensitivity ◽  
Bisphenol S ◽  
Milk Samples ◽  
Multiple Reaction Monitoring Mode ◽  
Sensitivity And Selectivity ◽  
Primary Secondary Amine ◽  
Array Detection

Abstract Different extraction and clean-up protocols, based on either the dispersive solid-phase extraction (d-SPE) and the quick, easy, cheap, effective, rugged, and safe (QuEChERS) approach, were optimized and compared for the determination of selected bisphenols such as bisphenol A (BPA) and bisphenol S (BPS) in breast milk samples. QuEChERS-based sample preparation procedure was optimized by evaluation of different clean-up sorbents including zirconium-based sorbents (Z-Sep and Z-Sep Plus) and primary secondary amine. Negligible matrix interference was observed for most of the analytes due to application of 45 mg Z-Sep or 45 mg Z-Sep + 5 mg Z-Sep Plus sorbents in d-SPE clean-up step. Acceptable analytical performance for the BPA and BPS was observed with recoveries percentage in the range of 70–92% and RSD less than 15%. The pilot study was performed by applying HPLC with diode-array detection, and optimized procedures were transferred to the LC triple-quadrupole MS system. LC with electrospray ionization and tandem MS operating in the multiple reaction monitoring mode provide high sensitivity and selectivity for trace analysis. The LODs were 0.10 and 0.54 ng/mL, and the LOQs were 0.20 and 1.35 ng/mL for BPS and BPA, respectively. The developed procedures were evaluated in terms for material collection obtained from women (inhabitants of Lublin, Poland). In 20 samples, bisphenol residues were detected at concentrations from 0.09 to 11.56 ng/mL.

Determination of Dufulin Residue in Vegetables, Rice, and Tobacco Using Liquid Chromatography with Tandem Mass Spectrometry

2015 ◽  
Vol 98 (6) ◽  
pp. 1739-1744 ◽  
Author(s):  
Yanjiao Li ◽  
Ping Lu ◽  
Deyu Hu ◽  
Pinaki S Bhadury ◽  
Yuping Zhang ◽  
...  
Keyword(s):  
Multiple Reaction Monitoring ◽  
Antiviral Agent ◽  
Graphitized Carbon Black ◽  
The Novel ◽  
Multiple Reaction Monitoring Mode ◽  
Primary Secondary Amine ◽  
Rice Samples ◽  
Dispersive Spe ◽  
Actual Trial

Abstract A rapid and accurate LC/MS/MS method using positive electrospray ionization was established for the determination of residues of the novel plant antiviral agent dufulin in samples of tobacco leaf (dry), tomato, cucumber, and rice. Samples were extracted with acetonitrile; cleaned up by dispersive SPE using primary secondary amine, C18, and graphitized carbon black sorbents; separated on a C18 column; and confirmed by multiple reaction monitoring mode MS with a matrix effect of –21.5–19.6%. The method showed satisfactory linearity (R2 ≥0.9912) for the target compound. The LOD and the LOQ were 0.05 and 0.15 μg/kg, respectively. The mean recoveries from four matrixes varied from 71.9 to 93.6% with intraday RSD in the range of 2.9 to 9.0% and interday RSD 6.9 to 15.2%. The method was successfully applied for analysis of dufulin in actual trial samples.

scholarly journals Portable smartphone-integrated paper sensors for fluorescence detection of As(III) in groundwater

2020 ◽  
Vol 7 (12) ◽  
pp. 201500
Author(s):  
Sha Liu ◽  
Yong Li ◽  
Chao Yang ◽  
Liqiang Lu ◽  
Yulun Nie ◽  
...  
Keyword(s):  
Environmental Problem ◽  
Visual Detection ◽  
High Sensitivity ◽  
Integration System ◽  
Detection Range ◽  
Sensitivity And Selectivity ◽  
Toxic Metalloid ◽  
Interfering Ions ◽  
Cu Nanoclusters

Arsenic contamination in groundwater is a supreme environmental problem, and levels of this toxic metalloid must be strictly monitored by a portable, sensitive and selective analytical device. Herein, a new system of smartphone-integrated paper sensors with Cu nanoclusters was established for the effective detection of As(III) in groundwater. For the integration system, the fluorescence emissive peak of Cu nanoclusters at 600 nm decreased gradually with increasing As(III) addition. Meanwhile, the fluorescence colour also changed from orange to colourless, and the detection limit was determined as 2.93 nM (0.22 ppb) in a wide detection range. The interfering ions also cannot influence the detection selectivity of As(III). Furthermore, the portable paper sensors based on Cu nanoclusters were fabricated for visual detection of As(III) in groundwater. The quantitative determination of As(III) in natural groundwater has also been accomplished with the aid of a common smartphone. Our work has provided a portable and on-site detection technique toward As(III) in groundwater with high sensitivity and selectivity.

scholarly journals Ultrasound-Assisted Solvent Extraction of a Porous Membrane Packed Sample for the Determination of Tobacco-Specific Nitrosamines in the Replacement Liquids for E-Cigarettes

Molecules ◽  
2019 ◽  
Vol 24 (24) ◽  
pp. 4618 ◽  
Author(s):  
Paweł Kubica
Keyword(s):  
Solvent Extraction ◽  
Sample Preparation ◽  
Electronic Cigarettes ◽  
Multiple Reaction Monitoring ◽  
Porous Membrane ◽  
Liquid Chromatography Tandem Mass ◽  
Multiple Reaction Monitoring Mode ◽  
Ultrasound Assisted ◽  
Tobacco Specific Nitrosamines

The content of tobacco-specific nitrosamines (TSNAs) possessing carcinogenic properties has been an important area of research since replacement liquids were introduced for e-cigarettes. A method for determining N′-nitrosonornicotine (NNN), 4-(methylnitrosamino)-1-(3-pyridyl)-1-butanone (NNK), N′-nitrosoanatabine (NAT), and N′-nitrosoanabasine (NAB) in replacement liquids for electronic cigarettes was developed using liquid chromatography–tandem mass spectrometry with electrospray ionisation (HPLC-ESI-MS/MS) in the multiple reaction monitoring mode. The sample preparation of replacement liquids was accomplished via the ultrasound-assisted solvent extraction of a porous membrane packed sample. The sample preparation proved to be successful in extracting the analytes, with recoveries from 87% to 105%, with coefficients of variation < 4.9%. Moreover, the linearity and limits of detection and quantitation (LOD, LOQ), together with repeatability and accuracy, were determined for the developed method. The proposed sample preparation and developed chromatographic method were successfully applied to the determination of TSNAs in 9 replacement liquid samples. The NNK and NNN were found to be most frequently detected (89 and 67%, respectively), with concentration ranges from 1.2–54.3 ng/mL and 4.1–30.2 ng/mL, respectively, while NAT was detected with frequency of 22% with range 1.7–2.5 ng/mL and NAB were found to be below the LOD in all samples.

Determination of butyltin and phenyltin analogues in sea products by Grignard derivatization and gas chromatography-triple quadrupole tandem mass spectrometry

2014 ◽  
Vol 6 (23) ◽  
pp. 9333-9339 ◽  
Author(s):  
Zongyan Cui ◽  
Yunkai Qian ◽  
Na Ge ◽  
Jinjie Zhang ◽  
Yongming Liu ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Tandem Mass Spectrometry ◽  
High Sensitivity ◽  
Tandem Mass ◽  
Triple Quadrupole ◽  
Sensitivity And Selectivity

A GC MS/MS method was development with high sensitivity and selectivity for organotin speciation in sea products.

scholarly journals Analytical considerations on the use of a fruit-specific and representative matrix in pesticide residue analysis by LC-ESI-MS/MS

2013 ◽  
Vol 11 (7) ◽  
pp. 1112-1131 ◽  
Author(s):  
Anna Stachniuk ◽  
Emilia Fornal
Keyword(s):  
Pesticide Residue ◽  
Calibration Curve ◽  
Multiple Reaction Monitoring ◽  
Residue Analysis ◽  
Pesticide Residue Analysis ◽  
Liquid Chromatography Mass Spectrometry ◽  
Black Currant ◽  
Relative Standard ◽  
Multiple Reaction Monitoring Mode ◽  
Analytical Errors

AbstractOne of the quantification methods frequently applied to pesticide residue analysis in food by liquid chromatography — mass spectrometry (LC-MS) involves matrix-matched calibrations with a representative matrix used for all commodities belonging to one group. This approach, although very practical, is deemed to generate analytical errors. The effect of the application of a representative-matrix calibration curve on the pesticide quantification result was examined. Extractions of 56 pesticides from five soft fruits (strawberries, blackberries, raspberries, black currant and red currant) were carried out using QuEChERS method. Pesticide determinations were performed by LC-MS/MS in multiple reaction monitoring mode. Quantification difference functions and parameters were proposed and calculated. At the concentration of 0.05 mg kg−1 for ca. 90% of examined pesticides the quantification difference arising from the use of a representative matrix calibration curve (raspberries) instead of a specific fruit matrix calibration curve was below 20% for black and red currents, and below 30% and 35% in the case of strawberries and blackberries, respectively. The 25% difference limit was not exceeded for 51 pesticides in black and red currents, 46 pesticides in blackberries and 45 pesticides in strawberries. Quantification difference functions and parameters such as relative standard deviation of corrected process efficiencies were found to be helpful in data-driven decision-making on the applicability of a representative matrix; the former may be also used as a tool for data correction to ensure the reliability and accuracy of analyses.

scholarly journals Exploring peptide capture by anti-protein antibodies for LC-MS-based biomarker determination

2018 ◽  
Author(s):  
Maren Levernæs ◽  
Bassem Farhat ◽  
Inger Oulie ◽  
Sazan S. Abdullah ◽  
Elisabeth Paus ◽  
...  
Keyword(s):  
Protein Extraction ◽  
High Sensitivity ◽  
Intact Protein ◽  
Protein Biomarkers ◽  
Promising Technique ◽  
Intact Proteins ◽  
Protein Levels ◽  
Endogenous Protein ◽  
Sensitivity And Selectivity

<p>Immunocapture LC-MS/MS is a promising technique to ensure high sensitivity and selectivity of low-abundant protein biomarkers. For this purpose, the use of monoclonal antibodies (mAb) is especially attractive as they are renewable reagents that can be standardized. In this article we investigated the possibility of using mAbs developed against intact proteins (anti-protein antibodies) to capture proteotypic epitope peptides. Three mAbs were tested, and all selectively extracted proteotypic epitope peptides from a complex sample. Compared to intact protein extraction, this concept which we call peptide capture by anti-protein antibodies provided cleaner extracts, which further improved the sensitivity. Analysis of three patient samples demonstrated that p can be used for the determination of different endogenous protein levels. </p><p></p>

scholarly journals Simultaneous LC-MS/MS Determination of Sacubitril, Valsartan and LBQ657 in Human Plasma and Its Application to Clinical Study

2021 ◽  
Author(s):  
Yufeng Ni ◽  
Yujia Zhang ◽  
Chong Zou ◽  
Li Ding
Keyword(s):  
Human Plasma ◽  
Multiple Reaction Monitoring ◽  
Gradient Elution ◽  
Ionization Source ◽  
Internal Standards ◽  
Accuracy And Precision ◽  
Liquid Chromatography Tandem Mass ◽  
Multiple Reaction Monitoring Mode ◽  
Positive Ion

A rapid and reproducible liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated to simultaneously determine sacubitril, valsartan and a metabolite of sacubitril (LBQ657) in human plasma using sacubitril-d4 and valsartan-d3 as the internal standards. Following protein precipitation, the analytes were operated on an Ultimate® XB-C18 column (2.1 × 50 mm, 3.5 μm, Welch) with a gradient elution with acetonitrile, and 5 mM ammonium acetate and 0.1% formic acid in water as the mobile phase. The detection was performed on a Triple Quad™ 4000 mass spectrometer coupled with an electrospray ionization source (ESI) under positive-ion multiple reaction monitoring mode. The linearities are 2.00-4000, 5.00-10000 and 5.00-10000 ng mL-1 for sacubitril, valsartan and LBQ657, respectively. The accuracy and precision of intra- and inter-day, dilution accuracy, recovery and stability of the method were all within the acceptable limits and no matrix effect or carryover was observed. The suitability of the method was successfully demonstrated in terms of the quantification of sacubitril, valsartan and LBQ657 in plasma samples collected from healthy Chinese volunteers in a clinical trial.

DBS Assay with LC-MS/MS for the Determination of Idelalisib, A Selective PI3K-δ Inhibitor in Mice Blood and Its Application to a Pharmacokinetic Study

Drug Research ◽  
2020 ◽  
Vol 71 (01) ◽  
pp. 36-42
Author(s):  
Harsha K. Tripathy ◽  
Nair S.V. Manju ◽  
Sreekanth Dittakavi ◽  
Ashok Zakkula ◽  
Ramesh Mullangi
Keyword(s):  
Pharmacokinetic Study ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Lymphocytic Leukemia ◽  
Extraction Solvent ◽  
Non Hodgkin Lymphoma ◽  
Validation Parameters ◽  
Multiple Reaction Monitoring Mode ◽  
Carry Over

AbstractIdelalisib is a selective and second-generation PI3K-δ inhibitor, approved for the treatment of non-Hodgkin lymphoma and chronic lymphocytic leukemia. In this paper, we present a fully validated dried blood spot (DBS) method for the quantitation of idelalisib from mice blood using an LC-MS/MS, which was operated under multiple reaction monitoring mode. To the punched DBS discs, acidified methanol enriched with internal standard (IS; larotrectinib) was added and extracted using tert-butyl methyl ether as an extraction solvent with sonication. Chromatographic separation of idelalisib and the IS was achieved on an Atlantis dC18 column using a mixture of 10 mM ammonium formate:acetonitrile (25:75, v/v). The flow-rate and injection volume were 0.80 mL/min and 2.0 µL, respectively. Idelalisib and the IS were eluted at ~0.98 and 0.93 min, respectively and the total run time was 2.00 min. Idelalisib and the IS were analyzed using positive ion scan mode and parent-daughter mass to charge ion (m/z) transition of 416.1→176.1 and 429.1→342.1, respectively was used for the quantitation. The calibration range was 1.01−4 797 ng/mL. No matrix effect and carry over were observed. Haematocrit did not influence DBS idelalisib concentrations. All the validation parameters met the acceptance criteria. The applicability of the validated method was shown in a mice pharmacokinetic study.

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