Pesticides and their metabolites are of great concern to our society as they are harmful to human health, pollute natural resources and disturb the equilibrium of the ecosystem. Consequently, stricter food safety regulations are being enforced around the world, placing pesticide analysis laboratories under increasing pressure to expand the list of targeted pesticides and detect analytes at lower and lower levels with high precision. National programs for pesticide monitoring in Europe, the US and Japan have set Maximum Residue Levels (MRL’s) or tolerance information (EPA) for monitoring the steadily increang number of pesticides in food products.


Expanding Capabilities in Multi-Residue Pesticide Analysis Using The LCMS-8060

Shimadzu offers a wide range of instruments/solutions for pesticide testing including LC, SFC, GC coupled with triple quadrupole mass spectrometers. LC-MS/MS MRM (Multiple Reaction Monitoring) analysis allows for rapid and sensitive detection of pesticides in complex matrices. A single multi-residue LC-MS/MS method was developed for 646 pesticides (3 MRM transitions for over 99 % targeted pesticides resulting in 1,919 transitions in total, with a polarity switching time of 5 msec) using Ultra-Fast LC-MS/MS and a Method Package for Residual Pesticides.


Fully automated derivatization and quantification of Glyphosate and AMPA in beer using a standard UHPLC-MS/MS system

Glyphosate is currently one of the most common pesticides used worldwide. In spite of its approval by regulatory bodies all over the world, the concern about its harm to humans and the environment persists. Therefore, the strict control of Glyphosate and its metabolite Aminomethylphosphonic acid (AMPA) in food and environment is mandatory. The chromatography of glyphosate is challenging due to its high polarity. In order to overcome this, there exists a well-established method including a derivatization step with 9-fluorenylmethyl chloroformate (FMOC) followed by LCMS analysis.

Shimadzu has developed a method using a fully automated derivatization followed by LC-MS/MS analysis. The instrumental set-up does not require any additional hardware for sample pretreatment but uses the built-in pretreatment function of the autosampler. The method has been evaluated using 40 commercially available beer samples. Analytical results are available here:

Evaluation of supercritical fluid chromatography (SFC) coupled to tandem mass spectrometry for pesticide residues in Food

Supercritical fluid chromatography coupled to triple quadrupole mass spectrometry (SFC-MS/MS) has been used for analysis of pesticide residues in food. A method has been developed for identification and quantitation of 164 pesticides in three differnt matrices tomato, orange and leek. This system configuration with Carbon dioxide as mobile phase and methanol as modifier is a good alternative to LC-MS/MS and is reducing matrix effects and shortening run times.

Sensitive method for the determination of Fipronil in egg using UHPLC-MS/MS [LCMS-8060]

Fipronil is a broad-spectrum insecticide used against fleas, lice, ticks, cockroaches, mites and other insects. The World Health Organization considers fipronil to be "moderately toxic" to humans. In large quantities it can damage the liver, kidneys and thyroid gland. The European regulations for the use of fipronil was adjusted on January 1st this year. Fipronil is now banned from being used in pesticides in high concentrations. The Federal Institute for risk assessment (BfR) in Berlin is reporting analysis results of fipronil levels in a range from 0.0031 to 1.2 mg per kg in chicken eggs, which is a health risk for children. Shimadzu has developed an ultra-sensitive and rapid assay of fipronil and some metabolites in food such as honey and more.

Ultra-Sensitive and Rapid Assay of Neonicotinoids, Fipronil and Some Metabolites in Honey by UHPLC-MS/MS [LCMS-8060]

Neonicotinoids are a class of insecticides widely used to protect fields as well as fruits and vegetables. Recently the use of this compounds became very controversial as they were pointed as one cause of the honeybees colony collapse disorder. Since pollination is essential for agriculture, extensive studies have been conducted to evaluate the impact of neonicotinoids on bee health. Following this the EFSA limited the use of thiamethoxam, clothianidin and imidacloprid. Fipronil, a pesticide from a different chemical class, has been also banned by EFSA for maize seed treatment due to its high risk for honeybee health. In order to better understand the effect of these compounds on bees and their contamination in pollen and honey, a highly sensitive assay method has been developed.

Highly sensitive Pesticide Residue analysis in food with GC-MS/MS Instrumentation using Hydrogen as Carrier Gas

Contamination of food products with pesticides is a growing concern because of recognized adverse health effects, increasing world-wide usage of pesticides, and increasing imports of raw foodstuffs from foreign sources. Consequently, the amount of monitored pesticides as well as the number of samples to be analyzed on GC-MS/MS became significantly higher in the last decade. A highly sensitive method has been developed on the GCMS-TQ8040 and the use of hydrogen as carrier gas for pesticide residue analysis was investigated on the basis of apple matrix spiked with 120 different pesticides. All compounds were detectable down to 5 ppb, calibration curves and correlation factors proved good linearity. At 10 ppb the %RSD values for many compounds were below 20%.

Simultaneous Analysis of Residual Pesticides in Foods via the QuEChERS Method Utilizing GC-MS/MS

The European Union Reference Laboratory (EURL) has reported their results on evaluating the validity of residual pesticide analysis utilizing GC-MS/MS and LC-MS/MS. In their report, the measurement of 66 pesiticides using GC-MS/MS was recommended. This data sheet presents selected results of analysis of these pesticides using the triple quadrupole GCMS-TQ8030.

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