Page 11 - Shimadzu Journal vol.1

Food safety . 11

LCMS-8040 triple quadrupole mass spectrometer ESI-Positive and negative (15 msec. polarity switch) Dwell time 5 msec. Pause time 1 msec. 250 o C 400 o C 15 L min -1 2 L min -1 1:1 water:methanol with 10 mM ammonium acetate Flow rate: 0.5mL min -1 Flow injection analysis (No column fitted) 0.2 μL (0.01 mg kg -1 pesticide standard solution) Carrier 1:1 water:methanol Flow rate: 0.3mL min -1 Flow injection analysis (No column fitted) 5 μL injection (0.01 mg kg -1 pesticide standard solution) 1 μL air gap (see text for mobile phase compositions) Pesticide limits of detection were calculated based on the method described by the US-EPA in Title 40 Code of Federal Regulation Part 136

MS Parameters MS: Ionisation: SRM: Desolvation line: Heating block: Drying gas: Nebulising gas: SRM optimisation: Mobile phase screening: interval: ( = analyses. 3. Results and discussion 3.1 SRM optimisation transitions are shown in Table-1.

ʢ5ʙ200ppbʣ Shim-pack XR-ODS III (150 x 2 mm, 2.2 µm A = Water with 5 mM ammonium formate and B = Methanol with 5 mM ammonium formate B% A% 5 95 100 0 100 0 5 95 5 95 32 µL (stacked injection: 2 µL sample + 30µL
In this work, we discuss the development of a multi-residue pesticide
addition to ensuring chromatographic resolution of pesticide isomers
discussed pitfalls of GCMS, have meant LCMSMS has become a vital
method for 210 pesticides using the Nexera UHPLC and LCMS-8040
preparation. The method was evaluated in matrix to ensure that the
regulatory guidelines around the world with acceptable precision, in
without the need for derivatisation. 9 Recent improvements in liquid
chromatography - tandem mass spectrometry, combined with the
selective and sensitive analysis and is well suited to the multi-class
necessary reporting limits were obtained according to the various
technique. LC-triple quadruple mass spectrometry enables highly
be analysed in this way due to poor thermal stability or volatility
triple quadruple. Pesticides were matrix-matched in food matrix
(lettuce, pear and dried fruit) following QuEChERS sample
analysis of large numbers of pesticides at trace levels.
with identical SRM transitions. 2. Experimental A stock of pesticides was obtained from the Food and Environment Agency, UK, at a concentration of 0.01 mg kg -1 (for each pesticide) in acetone:acetonitrile 1:1. Linearity was investigated over a nine-point calibration with samples ranging from 0.005ʙ0.2mgkg-1 analysed in duplicate; calibration samples were injected once in increasing order and once in decreasing order. Linearity was assessed with four calibration curves prepared by serial dilution of: (1) acetonitrile, (2) dried fruit extract, (3) lettuce extract and, (4) pear extract. Instrumental area repeatability was determined by replicate (n=6) injection

published national standard GB 2763-2005 in 2005 and more recently
analysis turnaround times, and all the while maintaining or reducing costs. In this study a method was successfully developed for the quantitation
reporting level was typically less than 5 %RSD for compounds and correlation coefficients were typically greater than 0.997 in a variety of studied
system for agricultural chemical residues in foods, introduced in 2006,
Dr. Simon Hird from the Food and Environment Research Agency (FERA) in York
of 210 commonly analysed pesticides in food samples using the Nexera UHPLC and LCMS-8040. Initial validation was performed to demonstrate
contains MRLs for over 400 pesticides in various commodities. 6 China
laboratories under increasing pressure to expand the list of targeted pesticides, detect analytes at lower levels and with greater precision, reduce
food extracts. Consequently, the LCMS-8040 is ideally suited for routine monitoring of pesticides below the 0.01 mg kg -1 default level set by EU
Regulations (US Environmental Protection Agency Office of Pesticide
Pesticides and their metabolites are of great concern to society as they are harmful to human health, pollute natural resources and disturb the
instrument capabilities. Limits of detection (LOD) for 90 % of compounds were less than 0.001 mg kg-1 (1 ppb) and all compounds were less
even lower MRLs for a few other very toxic pesticides. 4 Regulatory
guidelines. In the US, tolerances for more than 450 pesticides and
equilibrium of the ecosystem. Consequently, stricter food safety regulations are being enforced around the world, placing pesticide analysis
than 0.01 mg kg -1 (10 ppb) for both the quantifying and qualifying transitions using only a 2 µL injection. Repeatability at the 0.01 mg kg -1
Programs) and are enforced by the US FDA. 5 Japan’s positive list
bodies around the world, as in the EU, have produced similar
other ingredients are stated in the electronic Code of Federal
David R. Baker 1 , Chris Titman 1 , Alan J. Barnes 1 , Neil J. Loftus 1 , Alexander Mastoroudes 2 , Simon Hird 3
MRLS for 85 pesticides in food. 7,8 GB 28260-2011 which was introduced in 2012 and specifies 181 Consequently, pesticide analysis laboratories are under increasing pressure to expand the list of targeted pesticides, detect analytes at lower levels and with greater precision, reduce analysis turnaround times and reduce usage of hazardous solvents while maintaining or reducing costs. Pesticide residues were traditionally analysed mainly by GC-based multi-residue methods often with MS detection. However, many modern (semi)polar compounds and/or ionic compounds could not

global w430×h280 Multi-Residue Analysis of 210 Pesticides in Food Samples by Triple Quadrupole UHPLC-MS/MS 1 Shimadzu Corporation, Manchester, UK 2 Kings College London, London, UK 3 Food and Environment Research Agency, York, UK and Japanese legislation. Keywords : Pesticides; Multi-residue analysis; LCMS-8040; Food safety; Fruit; Vegetables Pesticide residues in food continue to be the target of studies due to the uncertainty concerning adverse effects that those residues may have on human health after a lengthy exposure at low levels. More than 1000 active ingredients have been utilised and are formulated in thousands of different commercial products. They include a variety of compounds, mainly insecticide

Food safety Abstract 1. Introduction pesticide. 2 10