scholarly journals Quantification and Confirmation of Fifteen Carbamate Pesticide Residues by Multiple Reaction Monitoring and Enhanced Product Ion Scan Modes via LC-MS/MS QTRAP System

Molecules ◽  
2018 ◽  
Vol 23 (10) ◽  
pp. 2496 ◽  
Author(s):  
Ying Zhou ◽  
Jian Guan ◽  
Weiwei Gao ◽  
Shencong Lv ◽  
Miaohua Ge

In this research, fifteen carbamate pesticide residues were systematically analyzed by ultra-high performance liquid chromatography–quadrupole-linear ion trap mass spectrometry on a QTRAP 5500 system in both multiple reaction monitoring (MRM) and enhanced product ion (EPI) scan modes. The carbamate pesticide residues were extracted from a variety of samples by QuEChERS method and separated by a popular reverse phase column (Waters BEH C18). Except for the current conformation criteria including selected ion pairs, retention time and relative intensities from MRM scan mode, the presence of carbamate pesticide residues in diverse samples, especially some doubtful cases, could also be confirmed by the matching of carbamate pesticide spectra via EPI scan mode. Moreover, the fragmentation routes of fifteen carbamates were firstly explained based on the mass spectra obtained by a QTRAP system; the characteristic fragment ion from a neutral loss of CH3NCO (−57 Da) could be observed. The limits of detection and quantification for fifteen carbamates were 0.2–2.0 μg kg−1 and 0.5–5.0 μg kg−1, respectively. For the intra- (n = 3) and inter-day (n = 15) precisions, the recoveries of fifteen carbamates from spiked samples ranged from 88.1% to 118.4%, and the coefficients of variation (CVs) were all below 10%. The method was applied to pesticide residues detection in fruit, vegetable and green tea samples taken from local markets, in which carbamates were extensively detected but all below the standard of maximum residue limit.

2020 ◽  
Vol 98 (Supplement_4) ◽  
pp. 362-363
Author(s):  
Daniil Khvostov ◽  
Natalya Vostrikova ◽  
Irina M Chernukha

Abstract Functional, particularly personalized meat-based foods are of more in demand by a consumer today. Functional additives, such as plant components and animal proteins from bovine or porcine tissues have been successfully used. With many ingredients added to foods, it is important to provide quality and composition monitoring to confirm the products’ authenticity, to identify undeclared or rarely used types of raw meat in product formulations. For example, if animal heart tissue is a component of a product formulation or if aorta tissue presents in a product due to improper trimming. Different methods are used to identify raw materials, including new approaches in proteomics and peptidomics that are considered the most effective modern methods nowadays. The purpose of the study is meat product composition analysis and special biomarker peptide identification to confirm the presence of heart and aorta tissue in a finished meat product. Over 20 amino acid sequences were checked based on earlier obtained data. Those amino acid sequences were analyzed with a high-performance liquid chromatography with mass spectrometric detection as described. The MS settings were selected using the Skyline. Signal-to-Noise ratio (S/N) over 10 units were used to choose the best peptide candidates. Seven peptides were found in porcine hearts. The best candidate was peptide VNVDEVGGEALGR (S/N - 73.10±5.3) from β-Hemoglobin. Two marker peptides from serum albumin were selected for pork aorta: TVLGNFAAFVQK (S/N 53.51±2.4) and EVTEFAK (S/N 31.69±4.1). These biomarkers showed the best detection and specificity. The multiply reaction monitoring method made it possible to identify the most/best specific peptides—biomarkers that could confirm the heart and/or aorta in meat products. The method can be used for comparative research or identification of best peptides that are specific to any type of animal tissue. The work was supported by the Russian Science Foundation, project no. 16-16- 10073.


2016 ◽  
Vol 99 (6) ◽  
pp. 1628-1635 ◽  
Author(s):  
Qianqian Sun ◽  
Yihu Wang ◽  
Chunxia Tian ◽  
Wenjun Gui ◽  
Yirong Guo ◽  
...  

Abstract A reliable and rapid method was developed to determine benzobicyclon residue in different soil and sediment samples. After extraction via a modified quick, easy, cheap, effective, rugged, and safe method, samples were purified by SPE cleanup with HLB cartridges. Quantitative determination was performed by ultra-HPLC (UPLC)-tandem MS (MS/MS) in electrospray positive ionization and multiple reaction monitoring modes. When samples were fortified at concentrations of 5, 50, and 500 µg/L, recoveries of 80.2 to 114.5% were obtained, with the repeatability (intraday RSDr) and reproducibility (interday RSDR) <14.1 and <21.4%, respectively. The instrumental LODs and LOQs for matrix-matched standards and the method LOQs for sample test were 0.19–1.34 μg/L, 0.64–4.48 μg/L, and 0.32–2.24 μg/kg, respectively. The linear range was 5–1000 μg/L (R2 > 0.99). The established UPLC-MS/MS method was applied in the detection of benzobicyclon in real soil samples, which were collected during the supervised field trial. Results showed that the maximum concentration of benzobicyclon in the soil was 4.87 mg/kg and its degradation half-life (t0.5) was 6.7 days. Generally, the proposed method could be an effective tool for controlling and monitoring the risks posed by benzobicyclon to human health and environmental safety.


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