A Complementary, Quantitative and Confirmatory Method to UHPLC/ESI Q-Orbitrap Screening based on UPHLC/ESI-MS/MS for Analysis of 416 Pesticides in Fruits and Vegetables

2021 ◽  
Author(s):  
Willis Chow ◽  
Daniel Leung ◽  
Jian Wang
Keyword(s):  
Pesticide Residues ◽  
High Performance ◽  
Fruits And Vegetables ◽  
Method Development ◽  
Multiple Reaction Monitoring ◽  
Extraction Procedure ◽  
Screening Methods ◽  
Intermediate Precision ◽  
Esi Ms ◽  
Measurement Uncertainties

Abstract Background Triple quadrupole (MS/MS) and high-resolution mass spectrometer (HRMS), coupled with ultra-high performance liquid chromatography (UHPLC) or gas chromatography (GC), are technologies used to analyse pesticide residues in fruits and vegetables. LC-MS/MS has been the gold standard for analysis of pesticides, offering reliable performance and sensitivity, while LC-HRMS is expanding in applications to serve as another benchmark. Method development and testing scope expansion are constantly required with new generation mass spectrometers. Objective This paper discusses the development and validation of a quantitative and confirmatory method that can analyse over 400 pesticide residues using state-of-the-art UHPLC/ESI-MS/MS system. Method Homogenized fruit and vegetable samples were fortified with pesticides and were extracted using a modified QuEChERS method. Samples were injected onto a UHPLC/ESI-MS/MS system, and data were acquired in multiple reaction monitoring mode. The method was validated using a nested experimental design, and was able to quantify and confirm 416 pesticide in fruits and vegetables. It was also complimentary to the UHPLC/ESI Q-Orbitrap quantitative and screening methods previously developed in the authors’ laboratory. Results The method demonstrated good performance. In all matrices, 92% of pesticides yielded recoveries between 81–110%, more than 95% of pesticides yielded intermediate precision ≤ 20%, and about 65% of pesticides yielded measurement uncertainties ≤ 20%, and 96% of pesticides yielded measurement uncertainties ≤ 50%. Highlights This method was developed using the same mobile phases, analytical columns, and extraction procedure, as UHPLC/ESI Q-Orbitrap methods. Extracts can be run on either system, streamlining monitoring programs and offering high sample throughput.

UHPLC/ESI Q-Orbitrap Quantitation of 655 Pesticide Residues in Fruits and Vegetables—A Companion to an nDATA Working Flow

2020 ◽  
Vol 103 (6) ◽  
pp. 1547-1559
Author(s):  
Jian Wang ◽  
Daniel Leung ◽  
Willis Chow ◽  
Jon W Wong ◽  
James Chang
Keyword(s):  
Pesticide Residues ◽  
High Performance ◽  
Fruits And Vegetables ◽  
Residue Analysis ◽  
Resolving Power ◽  
Intermediate Precision ◽  
Monitoring Programs ◽  
Routine Monitoring ◽  
Mass Resolving Power ◽  
Chromatographic Resolution

Abstract Background Effective and expansive methods for multiresidue pesticide analysis are desired for routine monitoring programs. These methods are complex, especially when several hundred pesticides are involved. Objective Two approaches to sort data and identify isomers and isobaric ions in pesticide mixtures were evaluated to determine whether they could be differentiated by mass resolving power and/or chromatographic resolution. Method This study presents an application of ultra-high performance liquid chromatography electrospray Q-Orbitrap mass spectrometry (UHPLC/ESI Q-Orbitrap) along with QuEChERS for the quantitation of 655 pesticide residues in fruits and vegetables. Results From the developed method, 94.7% of the 655 pesticides in fruits and 93.9% of those in vegetables had recoveries between 81% and 110%; 98.3% in both fruits and vegetables had an intermediate precision of ≤20%; and 97.7% in fruits or 97.4% in vegetables showed measurement uncertainty of ≤50%. When the retention time difference (ΔtR) of two isomers was ≥0.12 min, they were chromatographically resolved. Twenty five out of 35 pairs or groups of isomers were chromatographically separated (ΔtR ≥ 0.12 min), but 14 pairs were not resolved (ΔtR < 0.12 min). There were 493 pairs of pesticides with a mass-to-charge difference of <1 Da. Only one pair of isobaric ions could not be separated by mass and chromatographic resolution. Highlights UHPLC/ESI Q-Orbitrap along with QuEChERS sample preparation offers a practical quantitative companion method to a non-target data acquisition for target analysis workflow for pesticide residue analysis in routine monitoring programs for food safety.

scholarly journals Development and method validation for determination of 54 pesticides in Okra by LC-MS/MS analysis

2020 ◽  
Vol 11 (1) ◽  
pp. 985-992
Author(s):  
Hymavati Muppalla ◽  
Kiranmayi Peddi
Keyword(s):  
European Union ◽  
Pesticide Residues ◽  
High Performance ◽  
Limit Of Detection ◽  
Extraction Procedure ◽  
Mass Spectrometry Analysis ◽  
Limit Of Quantification ◽  
Spectrometry Analysis ◽  
Tandem Mass Spectrometry Analysis

The presence of pesticide residues in primary and derived agricultural products raises serious health concerns for consumers across the globe. The aim of the present study was to assess the level of pesticide residues in Okra in India. A multi-residue method for the quantification of fifty-four pesticides in okra is described in this work. The present study employed a modified quick, easy cheap, effective rugged and safe (QuEChERS) extraction procedure followed by UHPLC-MS/MS (Ultra-High-Performance Liquid Chromatography coupled to Tandem Mass Spectrometry) analysis. Validation of the method was according to the guidelines given by European Union SANCO/12571/2013. The levels of validation were 10.0, 50.0 and 100 µg kg-1. The following parameters such as linearity, the limit of detection (LOD) (nearer to 0.005 mg kg-1) and limit of quantification (LOQ) (nearer to 0.01 mg kg-1) were set to be acceptable. The trueness of the method for 54 pesticides in all Okra commodities was between 80-110% with satisfactory repeatability and within-run reproducibility except for the pesticide residues such as Thiamethoxam and Fenamidone. The measurement of uncertainty for each of the pesticide was below 50% and was estimated to be in the range of 5.37% - 10.71%, which meets the criteria established in the SANCO/12571/2013 document (European Union, 2013). This method is concluded to be applicable for the determination of pesticide residues in Okra.

Sensitive Determination of C-Alkylated Flavonoids by HPLC-ESI-MS/MS Using Multiple Reaction Monitoring Approach: Pseudarthria hookeri as a Case Study

2019 ◽  
Vol 57 (10) ◽  
pp. 944-949
Author(s):  
Ina Faraz ◽  
Arslan Ali ◽  
Faraz Ul Haq ◽  
Joseph Tchamgoue ◽  
Simeon F Kouam ◽  
...  
Keyword(s):  
Quality Control ◽  
Method Development ◽  
Control Method ◽  
Raw Materials ◽  
Multiple Reaction Monitoring ◽  
Herbal Medicines ◽  
Reaction Monitoring ◽  
Linear Calibration ◽  
Esi Ms ◽  
Plant Raw Materials

Abstract One of the major problems with the formulation of herbal medicines is the quality control of plant material to ensure its efficacy and safety. Quality control of medicinal plants requires analysis of many bioactive compounds present in the plant. C-alkylated flavonoids are an important bioactive subclass of flavonoids. A simple, rapid, sensitive and selective method is presented here for the quantification of bioactive C-alkylated flavonoids. This is the first quantitative method for analysis of C-alkylated flavonoids based on the multiple reaction monitoring (MRM) approach so far. This study focuses on method development for quantification of bioactive C-alkylated flavonoids. Quantification of a total of five C-alkylated flavonoids was done employing the MRM approach on an HPLC-QqQ-MS instrument. LODs and LOQs for quantified flavonoids were in the range of 0.41–1.32 and 1.23–3.96 ng/mL, respectively. Linear calibration curves between 25 and 1500 ng/mL were obtained with the regression coefficients of ≥0.996. Accuracy (% bias) and precision (% RSD) of the analyses were found to be less than 5%. Developed HPLC-ESI-MS/MS can be employed as a quality control method of plant raw materials.

scholarly journals Bioanalytical Method Development and Validation of Memantine in Human Plasma by High Performance Liquid Chromatography with Tandem Mass Spectrometry: Application to Bioequivalence Study

2012 ◽  
Vol 2012 ◽  
pp. 1-8 ◽  
Author(s):  
Ravi Kumar Konda ◽  
B. R. Challa ◽  
Babu Rao Chandu ◽  
Kothapalli B. Chandrasekhar
Keyword(s):  
Human Plasma ◽  
High Performance ◽  
Method Development ◽  
Dynamic Range ◽  
Quantitative Estimation ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Bioequivalence Study ◽  
Healthy Human ◽  
Development And Validation

A simple, sensitive, and rapid HPLC-MS/MS method was developed and validated for quantitative estimation of memantine in human plasma. Chromatography was performed on Zorbax SB-C18(4.6×75 mm, 3.5 μm) column. Memantine (ME) and internal standard Memantine-d6(MED6) were extracted by using liquid-liquid extraction and analyzed by LC-ESI-MS/MS using multiple-reaction monitoring (MRM) mode. The assay exhibited a linear dynamic range of 50.00–50000.00 pg/ml for ME in human plasma. This method demonstrated an intra- and interday precision within the range of 2.1–3.7 and 1.4–7.8%, respectively. Further intra- and interday accuracy was within the range of 95.6–99.8 and 95.7–99.1% correspondingly. The mean recovery of ME and MED6 was86.07±6.87and80.31±5.70%, respectively. The described method was successfully employed in bioequivalence study of ME in Indian male healthy human volunteers under fasting conditions.

scholarly journals Monitoring of Pesticide Residues in Imported Fruits and Vegetables in United Arab Emirates during 2019

2021 ◽  
pp. 239-260
Author(s):  
Nasra M. Abd El- Mageed ◽  
Ideisan I. Abu- Abdoun ◽  
Abdulla S. Janaan
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
United Arab Emirates ◽  
Pesticide Residues ◽  
Fruits And Vegetables ◽  
Multiple Reaction Monitoring ◽  
Continuous Process ◽  
Tandem Mass

An accurate, rapid and reliable method for the simultaneous determination of pesticide multi-residues in 9724 samples imported fresh fruits and vegetables by a method of  liquid chromatography coupled with tandem mass spectrometry LC–ESI (+)-MS/MS operating in multiple reaction monitoring (MRM) mode, two transitions for each compound in the presence of internal standards and modified quick, easy, cheap, effective, rugged, safe (QuEChERS) method was used for the determination of 343 pesticides. The performance of the analytical method was validated in accordance with EU SANCO guidelines (SANTE/12682/2019) for monitoring pesticide multi-residues. Residues of 93 compounds, mainly fungicides and insecticides, were detected in 3548 samples. In this article, The potential applications of Liquid Chromatography and Tandem Mass spectrometry (MS/MS) techniques on monitoring pesticide residues of target samples of imported fruits and vegetables in United Arab Emirates (UAE) during the year 2019 is reported. The need for a continuous monitoring program of pesticide residues in imported fruits and vegetables is highly recommended and continuous process control for health and safety practices and to adhere to international agricultural and environmental policies of the country.

scholarly journals An LLE Based LC- ESI MS/MS Analytical Method Development to Detect Azithromycin Residue in Water to Monitor Contamination Level of River and Fish Farm of Bangladesh

2021 ◽  
Author(s):  
Md Humayun Kabir ◽  
Sabina Yasmin ◽  
Salma Akter Mou ◽  
Bushra Parvin Upoma ◽  
Shamim Ahmed ◽  
...  
Keyword(s):  
Analytical Method ◽  
Method Development ◽  
Limit Of Detection ◽  
Multiple Reaction Monitoring ◽  
Fish Farm ◽  
Contamination Level ◽  
Limit Of Quantification ◽  
Chromatographic Separations ◽  
Esi Ms ◽  
Multiple Reaction Monitoring Mode

Abstract The aim of this study to development and validate an analytical method to determine the Azithromycin (AZN) residue in water approach to monitor the contamination level of river and fish farm water of Bangladesh. Azithromycin (AZN) was analyzed using liquid chromatography mass spectrometry (LC-ESI MS/MS). The chromatographic separations of analyte were performed using ZORBAX RRHD Eclipse Plus C18 (2.1×100 mm, particle size 1.8 µm) column and mobile phase was 0.1% formic acid in water and acetonitrile with 50:50. The analyte were detected in positive electron spray ionization mode with multiple reaction monitoring mode (MRM) with mass transition from 749.5 m/z to 591 m/z and 158 m/z as quantifier and qualifier ion respectively. Liquid-liquid extraction method was used for the extraction of AZN residues. The developed method was validated in terms of accuracy, precision, linearity and specificity. The analyte showed a good linear in the range of 0.1-100 µg/L. Three spiking levels (0.25, 0.5 and 1.25 µg/L) was performed for determining accuracy and precision. Recoveries and RSD were in the range of 96.6-101.5% and 3.5-6.3 respectively. The estimated limit of detection and limit of quantification was 0.017 and 0.05 µg/L respectively. Using the developed method, we analyzed 5 different rivers and 5 different fish farm samples. We found no azithromycin residue in rivers water, but we found in one fish farm water azithromycin residue 0.35±0.06 µg/L. The results indicate that we should be concern to use antibiotics in fish farm water in different ways.

scholarly journals Quantitative analysis of fresh tomatoes (Solanum lycopersicum) for trace of pesticide residues from markets in Peshawar, Pakistan, using High Performance Thin Liquid Chromatography technique

2020 ◽  
Vol 23 (3) ◽  
pp. 708-714
Author(s):  
Syeda Kokab Shah ◽  
Syeda Faryal Israr ◽  
Asif Khan Khatak ◽  
Abeer Kazmi ◽  
Amir Ali ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Solanum Lycopersicum ◽  
Pesticide Residues ◽  
High Performance ◽  
Fruits And Vegetables ◽  
Phase 1 ◽  
Research Work ◽  
Efficient Approach ◽  
Maximum Residue Levels ◽  
Residue Levels

Background: Vegetables and fruits are vital constituents of human diet, as it provides necessary minerals and nutrients to human body to carry out biological reactions and provide protection against various diseases and injuries. Solanum lycopersicum (tomato) is consider as cash crop in Asian countries and are fine source of vitamin C, potassium, folate, vitamin K, and other bioactive compounds including, phenolics, flavonoids, carotenoids, and alkaloids. Similar to other crops, tomato quality and yield is also affected by pests. Globally, approximately 37.8% of tomato yield is spoiled due to pests. To maintain the vegetable quality and attain more yield, pest management approaches are applied, though extensive use of toxic pesticides are becoming a part of our food chain and causing adverse effects. Methodology: The present research is intended to evaluate the levels of toxic pesticides in different tomato varieties collected from four vegetable markets (Hayatabad Phase 1, Chargano Chowk, Kohat Road and Tarnab farm) in Peshawar, Pakistan. After collection of tomato samples, level of pesticide residues (Cyhalothrin, Cypermethrin, Chlorpyrifos, Bifenthrin, and Imidacloprid) were detected using high performance thin liquid Chromatography (HPTLC). Results: After detection, level of pesticides in sample was compared with Maximum residue levels (MRLs). The magnitude of pesticides in samples was lesser to the Maximum residue levels (MRLs) provided by United State Drug Agency (USDA), though the quantity of Lambda Cyhalothrin present in the sample was almost equal to MRL (0.097 mg/kg). Conclusion: HPTLC is an efficient approach to detect pesticide traces in fruits and vegetables. Research work should be focused on it, to identify and control farmer practices which are highly linked to pesticide contamination in tomatoes and use of biopesticides should be encouraged. The cultivation of transgenic tomatoes can also be an efficient approach to elude the utilization of toxic pesticides.

scholarly journals BIOANALYTICAL METHOD DEVELOPMENT AND VALIDATION OF ENTRECTINIB IN RAT PLASMA BY LIQUID CHROMATOGRAPHY–TANDEM MASS SPECTROMETRY

2020 ◽  
pp. 155-163
Author(s):  
PRAVALLIKA KE ◽  
PRAMEELA RANI A ◽  
RATNA KUMAR M
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
High Performance ◽  
Method Development ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Rat Plasma ◽  
Array Detector ◽  
Pharmaceutical Drugs ◽  
Relative Standard

Objective: The objective of the study was to develop and validate the bioanalytical liquid chromatography–mass spectrometry (LCMS/MS) method for the estimation of entrectinib in bulk and pharmaceutical drugs in rat plasma. Methods: Chromatographic separation of entrectinib with D4-entrectinib as internal standard (IS) was achieved using Waters Alliance high-performance liquid chromatography system, quaternary gradient pump of e2695, using Luna, 250×4.6 mm, 5 μm column and the mobile phase containing 0.1% formic acid and acetonitrile (ACN) within the ratio of 70:30% v/v. The flow was 1.0 ml/min; detection was carried out by absorption at 294 nm using a photodiode array detector at ambient temperature. Results: The peak of entrectinib was eluted at retention times of 5.225 min. The multiple reaction monitoring was 560.6/475.1 (m/z) for entrectinib and 580.6/496.3 (m/z) for IS entrectinib (D4). The linearity range was 1–20 ng/ml with a regression coefficient of 0.999. % relative standard deviation of peak areas of all measurements always <2.0. Conclusion: The method was successfully validated and it had been found to be within limits for accuracy, precision, and linearity and it is stable under analytical conditions used.

Sign in / Sign up

Export Citation Format

Share Document