Multiresidue Analysis of Pesticides in Moringa Pods by GC-MS/MS and LC-MS/MS

2020 ◽  
Vol 103 (6) ◽  
pp. 1486-1497
Author(s):  
Anirban Dutta ◽  
Sandip Hingmire ◽  
Kaushik Banerjee
Keyword(s):  
Mass Spectrometry ◽  
Tandem Mass Spectrometry ◽  
Ethyl Acetate ◽  
Large Scale ◽  
Tandem Mass ◽  
Multiresidue Analysis ◽  
Method Performance ◽  
Chromatography Tandem Mass Spectrometry ◽  
Ms Analysis ◽  
Accuracy And Precision

Abstract Background Moringa pods are known for their nutritional and health benefits. The cultivation of this crop receives frequent pesticide applications. In the absence of risk assessment data, maximum residue limits of pesticides in this crop are considered at the default level (0.01 mg/kg). However, there exists scarcely any validated method for pesticide residue analysis in this matrix. Objective This study was undertaken to develop and validate a multiresidue method for the simultaneous analysis of multi-class pesticides in moringa pods by gas chromatography-tandem mass spectrometry (GC-MS/MS), and liquid chromatography-tandem mass spectrometry (LC-MS/MS). Method The homogenized sample (10 g) was extracted with acetonitrile (10 mL). The extract was cleaned by dispersive solid-phase extraction using a combination of 50 mg primary secondary amine, 5 mg graphitized carbon black, and 25 mg C18 sorbents, and was directly analyzed by LC-MS/MS. Another portion of the extract was reconstituted in ethyl acetate before GC-MS/MS analysis. The method was validated as per the SANTE/12682/2019 guidelines using GC-MS/MS (180 pesticides) and LC-MS/MS instruments (203 pesticides). Results The method provided a satisfactory analysis of the targeted pesticides with good calibration linearity (r2>0.99), high precision (RSD < 20%), and accuracy (recoveries, 70 to 120%). The reconstitution of the acetonitrile extract in ethyl acetate significantly reduced the matrix effects on GC-MS/MS analysis. The use of matrix-matched standards could correct all recoveries. Conclusions The method offered a large-scale analysis of multi-class pesticides with high accuracy, and precision at 10 ng/g, and higher levels. The method performance complied with the regulatory requirements, and thus, can be implemented in routine testing purposes. Highlights The study reports a validated method for large-scale multiresidue analysis of pesticides in moringa matrix for the first time. The method provided a high throughput analysis of multi-class pesticides with satisfactory selectivity, sensitivity, accuracy, and precision.

scholarly journals PATH-19. TUMOR HETEROGENEITY IN GLIOMAS: A PILOT STUDY OF HISTOPATHOLOGY-ASSOCIATED PROTEOME PROFILES ASSESSED BY LIQUID CHROMATOGRAPHY TANDEM MASS SPECTROMETRY OF FFPE SAMPLES

2019 ◽  
Vol 21 (Supplement_6) ◽  
pp. vi147-vi147
Author(s):  
Aline Paixao Becker ◽  
Erica Hlavin Bell ◽  
S Jaharul Haque ◽  
Joseph McElroy ◽  
Jessica Fleming ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Tumor Heterogeneity ◽  
High Expression ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Ms Analysis ◽  
Ffpe Samples ◽  
Liquid Chromatography Tandem Mass

Abstract Herein, we aimed to scrutinize tumor heterogeneity of infiltrative gliomas based on histopathological phenotypes, through proteomic profiling of formalin-fixed, paraffin embedded (FFPE) tissue. FFPE tissues are promising samples for proteomic studies, which can support the elucidation of glioma evolution and identify therapeutically vulnerable proteins and signaling pathways that drive recurrence and resistance mechanisms. We represented 2–3 adjacent, phenotypically distinct areas from 12 grade II-IV gliomas diagnosed according to the 2016 WHO classification, in a total of 35 samples (1.0mm cores), that were analyzed employing liquid chromatography tandem mass spectrometry (LC-MS/MS) for label-free expression proteomics. The statistical analysis was performed using R and Qlucore™ omics explorer software. Overall, 9222 peptides were mapped to 1758 non-redundant proteins, 320 of which had a significant (p< 0.05) differential expression in glioblastomas versus lower grade gliomas (Wilcoxon test comparing average expression). Principal component analysis (PCA) of the whole set of proteins showed clustering of the samples by tumor grade and IDH status. Unsupervised hierarchical analysis of the most significantly expressed proteins (p= 0.01, FDR= 0.05) showed that IDHwt gliomas had high expression of proteins related to cell movement, DNA structure, and fatty acid metabolism throughout the samples. IDHmut gliomas largely displayed high expression of mitochondrial enzymes related to energy production and neurotransmitter metabolism, with subsets closely related to 1p19q status and histological grade. Importantly, we demonstrated that LC-MS/MS analysis of FFPE core samples is feasible and enables recognition of different proteome signatures across histopathological phenotypes within a single tumor. This is the first study, to our knowledge, exploring proteome profiles addressing histopathological heterogeneity in gliomas by LC-MS/MS analysis of FFPE samples, which warrants further validation in independent datasets including ones that utilize frozen specimens. FUNDING: R01CA108633, R01CA169368, RC2CA148190, U10CA180850-01 (NCI), Brain Tumor Funders Collaborative Grant, and the Ohio State University CCC (all to AC).

Application of Enzyme Digestion and Deconjugation Followed by Quick, Easy, Cheap, Effective, Rugged, Safe Extraction and Liquid Chromatography–Tandem Mass Spectrometry Methodology To Determine Ractopamine Residue in Pork

2018 ◽  
Vol 81 (8) ◽  
pp. 1258-1263 ◽  
Author(s):  
VANESSA GRESSLER ◽  
VIVIAN FEDDERN ◽  
JANE de OLIVEIRA PEIXOTO ◽  
MONICA CORREA LEDUR ◽  
OSMAR ANTONIO DALLA COSTA ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Sequential Analysis ◽  
Limit Of Detection ◽  
Residue Analysis ◽  
Tandem Mass ◽  
Method Performance ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass

ABSTRACT A new methodology is proposed for ractopamine residue analysis in pork. It consists of enzyme-mediated digestion and deconjugation steps; modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction; and liquid chromatography–tandem mass spectrometry (LC-MS/MS). In brief, the samples were digested with protease and then deconjugated with β-glucuronidase enzyme; they were then subjected to extraction and cleanup by QuEChERS and underwent sequential analysis by LC-MS/MS. The method performance was evaluated in accordance to the validation guidelines regulated by the Brazilian Ministry of Agriculture and Food Supply. The limit of detection was 0.15 μg/kg and limit of quantification was 0.5 μg/kg. When the method was applied to real samples, ractopamine residue was found in concentrations (up to 7.86 μg/kg) below international recommendation limits up to 10 μg/kg. The method is sensitive, accurate, quick, simple, and suitable for routine analysis; therefore, it is a monitoring tool that may be adopted by laboratories to achieve compliance levels.

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