Page 16 - Application Notebook - Solution for Food Safety

LAAN-A-LM-E107

Application Liquid Chromatography Mass Spectrometry

News Expanding Capabilities in Multi-Residue

Pesticide Analysis Using The LCMS-8060
No.C136 David R. Baker , Laëtitia Fages , Eric Capodanno , Neil Loftus 1
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Shimadzu Corporation, UK; Phytocontrol, France
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n Abstract was quickly and efficiently set up using the Shimadzu
With an increasing global population, food security is Pesticide MRM Library. For each target pesticide
increasingly under threat and there is a growing analysis, up to 3 MRMs (Multiple Reaction
challenge for agriculture to produce more food, safely Monitoring) transitions were imported from the
and more sustainably. The use of herbicides, library. 3 MRMs transitions provided additional data
insecticides, and fungicides reduce crop losses both confidence in reporting results in comparison to the
before and after harvest, and increase crop yields. conventional 2 transitions used in most methods. As
However, pesticide residues resulting from the use of the LCMS-8060 has a high data acquisition speed
plant protection products on crops may pose a risk to 1,919 transitions were acquired using a polarity
human health and require a legislative framework to switching speed of 5 msec over a 10.5 minutes
monitor pesticide residues in food. gradient elution.
National programs for pesticide monitoring in the US, To evaluate the method QuEChERS extracts of mint,
Europe and Japan have set Maximum Residue Levels tomato and apple were provided by a commercial
(MRL’s) or tolerance information (EPA) for pesticides in laboratory as raw acetonitrile extracts and spiked
food products. A default value of 0.01 mg/kg is applied with 646 pesticides (data is presented on the mint
for MRL enforcement, which therefore requires highly extract as it is the more complex sample matrix). The
sensitive and specific analytical technologies to monitor method was evaluated in matrix to ensure that the
an increasing number of pesticides. reporting limits were in agreement with recognised
This application note describes the expanded capability MRL’s.
of the LCMS-8060 to help accelerate method n Experiment
development workflows and support increased
pesticide monitoring programs. Using the Shimadzu Food extracts of mint, tomato and apple were
Pesticide MRM Library (the Library includes information supplied by Phytocontrol, France, following
on 766 certified reference materials) a single multi- established QuEChERS protocols. Final extracts were
residue LC/MS/MS method was developed for 646 prepared in acetonitrile without any dilution.
pesticides (3 MRM transitions for over 99 % targeted Certified reference materials for the Shimadzu
pesticides resulting in 1,919 transitions in total, with a Pesticide MRM Library were obtained from ACSD,
polarity switching time of 5 msec). France as stock solutions. All solvents were of LCMS
quality purchased from Sigma-Aldrich.
Keywords: Pesticides; food safety; LCMS-8060; A six point calibration curve from 0.002 - 0.1 mg/kg
Pesticide MRM Library, 776 compound (2 - 100 pg/μL) were generated using internal
library standard method. Two inter nal standards
(Atrazine-d5 and Diuron-d6) were spiked in during
n Introduction the auto-sampler sequence for quantitation.
There are more than 1,000 pesticides used globally The robustness of the LCMS-8060 was assessed by
on soil and crops. W ith the ever increasing peak area response for 646 pesticides spiked into
international trade of the food industry, regulatory mint, tomato and apple matrix extracts at 0.05 mg/kg.
bodies around the world have increased the number n LC/MS/MS method development
of regulated pesticides and the maximum residue
levels (MRLs) allowed in food commodities. In the EU, The Shimadzu Pesticide MRM Library has 766 pesticides
regulation 396/2005/EC and its annexes set MRLs for in its database (Application News No. C135). For each
over 500 pesticides in 370 food products. In the US, pesticide several MRM’s are included in the database
1)
tolerances for more than 450 pesticides and other and in this analysis the default value used was 3
2)
ingredients are established by the US EPA and MRM’s. For this method, 1,919 transitions were
Japan’s positive list system for agricultural chemical selected in both positive and negative ionisation mode
residues in foods contains MRLs for over 400 using a switching time of 5 msec (1,819 MRM
pesticides in various commodities. 3) transitions were in positive mode and 100 MRM
National pesticide monitoring programs create new transitions in negative mode).
challenges for food safety laboratories as the number To optimize ion source conditions (for example, DL
of pesticides required for analysis is increasing temperature, interface temperature, heating block
together with an expanded range of food products. temperature, heating gas flow, drying gas flow and
In this application paper we present the development nebulizer gas flow) the interface setting software was
of a LC-MS/MS method for screening and quantifying used. This tool provides an optimized response for all
over 646 pesticides in a single method. The method compounds.