Compensation of Matrix Effects by Postcolumn Infusion of a Monitor Substance in Multiresidue Analysis with LC−MS/MS

2009 ◽  
Vol 81 (6) ◽  
pp. 2185-2192 ◽  
Author(s):  
Helen Stahnke ◽  
Thorsten Reemtsma ◽  
Lutz Alder
2002 ◽  
Vol 966 (1-2) ◽  
pp. 155-165 ◽  
Author(s):  
F.J Egea González ◽  
M.E Hernández Torres ◽  
E Almansa López ◽  
L Cuadros-Rodrı́guez ◽  
J.L Martı́nez Vidal

2017 ◽  
Vol 100 (3) ◽  
pp. 616-623 ◽  
Author(s):  
Suchi Chawla ◽  
Hemlatta K Patel ◽  
Hetal N Gor ◽  
Kiran M Vaghela ◽  
Priti P Solanki ◽  
...  

Abstract The study was conducted to investigate matrix interferences using QuEChERS sample preparation to understandwhether the dilution of matrix and/or the grouping of commodities can eliminate the need for selective individual matrix-matched standards in LC with tandem MS (MS/MS) analysis, and whether the calibration graph based ononly one matrix can be used for quantification in the other matrixes. Matrix effects (MEs) were studied by comparing the slopes of calibration curves of the matrix-matched standards (diluted with mobile phase) vis-à-vis the solvent-based standards.The present study showed that MEs were dependent on the nature of both the commodity and the analyte. Among the test matrixes, the highest variability in ME was recorded in capsicum. Most of the pesticides showed signal suppression in tomato, capsicum, and cumin matrixes. In brinjal matrix,the signal of most of the pesticides showed slight enhancement. Due to the similar nature of the MEs in tomatoand capsicum, these two commodities can be grouped together. Considering analyte variability, acetamiprid, 3-hydroxy carbofuran, dichlorvos, dimethoate, and spinosyn A and D showed no significant ME (≤20%) in tomato. Very high MEs (2360.9 and 1250.8%) were observed for quizalofop-p-tefuryl and tebuconazole, respectively. To check the effect of dilution in minimizing the ME, cucumber and brinjal matrixes were diluted 10×, and calibration curves were drawn with five concentration levels. It was found that about 60% of the total analyzedpesticides showed MEs ≤20%. In cumin, MEs ranged from −5.3% for triazophos to 661% for thiacloprid. Most of the pesticides showed recoveries in the acceptable range of 70–130% with calibration curvesfrom both matrixes. To compensate for MEs, it is suggested that (1) tomato and capsicum matrixes, which show similar trends, can be grouped together; and (2) cucumber matrix, when diluted 10×, can be used to prepare calibration curves for the quantification of pesticides in various fruiting and cucurbit vegetable matrixes by LC-MS/MS.


2016 ◽  
Vol 5 (03) ◽  
pp. 4862 ◽  
Author(s):  
Mathew George* ◽  
Lincy Joseph ◽  
Arpit Kumar Jain ◽  
Anju V.

A simple, sensitive, rapid and economic high performance thin layer chromatographic method and a mass spectroscopic assay method has been developed for the quantification of telmisartan and hydrochlorthiazide combination in human plasma. The internal standards and analytes were extracted from human plasma by solid-phase extraction with HLB Oasis1cc (30mg) catridges. The scanning and optimization for the samples are done using methanol: water (50:50). The samples were chromatographed using reverse phase chromatography with C-18 column of different manufacturers like Ascentis C18 (150×4. 6, 5µ) using the buffer system Acetonitrile: Buffer (80:20%v/v) which consist of 2±0. 1Mm ammonium format at a flow rate of 0. 7ml/min at a column oven temperature 35±10c. The internal standard used was hydrochlorthiazide13c1, d2 and telmisartand3. The extraction techniques include conditioning, loading, washing and elution, drying followed by reconstitution of the dried samples. The volume injected was 10µl with the retention time of 3-4 min for telmisartan, 1-2 min for hydrochlorthiazide and for the internal standards the retention time was 3-4 min for telmisartand3 and 1-2 min for hydrochlorthiazide c13d2. The rinsing solution was Acetonitrile: HPLC grade water in the ratio (50:50). The above developed method was validated using various parameters like selectivity and sensitivity, accuracy and precision, matrix effects, % recovery and various stability studies. The method was proved to be sensitive, accurate, precise and reproducible. The preparation showed high recovery for the quantitative determination of telmisartan and hydrochlorthiazide in human plasma.


Metabolites ◽  
2021 ◽  
Vol 11 (1) ◽  
pp. 47
Author(s):  
Kourosh Hooshmand ◽  
Inge S. Fomsgaard

Glucosinolates are biologically active secondary metabolites in Brassicaceae plants that play a critical role in positive and negative interactions between plants and root-associated microbial communities. The aim of this study was to develop a reversed-phase liquid chromatography method to quantify and identify intact glucosinolates in the root of Arabidopsis thaliana (Arabidopsis) grown in non-sterile natural soil by using liquid chromatography-hybrid triple quadruple-linear ion trap (LC-QqQ(LIT)) mass spectrometry. The Synergi Fusion C18-based column was found to be effective for sufficient retention and separation of nine intact glucosinolates without the need for time-consuming desulfation or ion-pairing steps. Method validation results showed satisfactory inter-day and intra-day precision for all glucosinolates except for 4-hydroxyglucobrassicin. Good inter-day and intra-day accuracy and recovery results were observed for glucoiberin, gluconapin, glucobrassicin, 4-methoxyglucobrassicin and neoglucobrassicin. However, for 4-hydroxyglucobrassicin, glucoraphanin and glucoerucin corrections to quantification results might be necessary since the recovery and accuracy results were not optimal. Matrix effects were shown to have a negligible effect on the ionization of all target analytes. The established liquid chromatography–tandem mass spectrometry (LC-MS/MS) method was applied to quantify target intact glucosinolates in Arabidopsis root crude extract of four different wild-type accessions where differences in terms of concentration and composition of intact glucosinolates were observed. Employment of sensitive and selective precursor ion survey scan of m/z 97 in combination with the information-dependent acquisition (IDA) of the enhanced product ion (EPI) dependent scan (Prec97-IDA-EPI) using LC-QqQ(LIT) provided high confidence in structural characterization of diverse intact glucosinolate profiles in complex Arabidopsis root crude extract.


2020 ◽  
Vol 35 (4) ◽  
pp. 577-588
Author(s):  
Sebastian España Orozco ◽  
Philipp Zeitlinger ◽  
Karin Fackler ◽  
Robert H. Bischof ◽  
Antje Potthast

AbstractThe extraction of lipophilic wood extractives from pulp and paper process waters proves to be a challenging task, due to harsh and alternating process and sample conditions. This study has determined the potential use of polymeric sorbents for solid-phase extraction (SPE) and compared to classical silica-based reversed-phase packed columns, with polymeric hydrophilic-lipophilic balanced (HLB) cartridges being the sorbent with the most potential. Recovery functions were obtained with an internal standard mixture representative for the main lipophilic wood extractive groups, which are fatty acids and alcohols, sterols, sterol esters and triglycerides. The impact of pH, sample volume and sample matrix, expressed as TOC and cations, on the retention behavior of lipophilic extractives during SPE of industrial samples were determined with polymeric HLB sorbent. High variations in the composition of pulp mill matrices led to different optimal extraction conditions. Thus, a new SPE protocol was developed, which bypasses matrix interferences and omits the loss of analytes due to sample preparation. The method is applicable to different pulp mill effluents with large discrepancies in pH and sample matrices, resulting in recoveries >90 % with RSD <5 % for all lipophilic wood extractives.


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