Pesticide, Mycotoxins & Other Contaminates

LCMS-8040 Application - Screening Pesticides in Foods with DCBI
In this study, we attempted to develop a DCBI-MS approach to determine pesticides amount aiming at high throughput and comprehensive methods using MRM acquisition. Ambient mass spectrometry coupled with ultra-fast triple quadrupole mass spectrometry permits this data acquisition in 30 seconds per sample as compared with the conventional chromatographic run of about 20 - 40 minutes.
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LCMS-8045 Application - Highly Sensitive and Rapid Analysis of Synthetic Dyes in Sea Food by LC/MS/MS
Here, LC/MS/MS method has been developed for quantitation of malachite green, leucomalachite green, crystal violet and leucocrystal violet from sea food sample using LCMS-8045, a triple quadrupole mass spectrometer from Shimadzu Corporation, Japan.
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LCMS-8050 Application - Solid Phase Extraction and SFC-MS/MS Method for Analysis of Aflatoxins M1, M2, B1, B2, G1, and G2 in Milk Powders
A SFC-MS/MS analytical method is developed for quantitative analysis of a atoxins M1, M2, B1, B2, G1 and G2 in milk powders. A special sample preparation procedure is adopted, which includes extraction with adding of Q-Sep extract salt and puri cation with Supel™ Tox Alfazea SPE cartridge. This new procedure was proven to be ef cient in extraction of the six a atoxins in milk powders and in the subsequent puri cation for high sensitivity MRM based analysis method. The LOQs of the method for the six a atoxins is at 22.8~68.0 ng/kg for a atoxin B1, B2, G1 and G2, and are 30.0 ng/kg and 34.4 ng/kg for a atoxin M1 and M2, respectively.
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LCMS-8060 Application - Application of SFC-MS/MS for the quantification of highly polar pesticides in a range of food samples
The analysis of highly polar pesticides by LC-MS/MS is typically achieved by several specific methods with limited chemical space. The EU Reference Laboratories for Residues of Pesticides Single Residue Methods (EURL-SRM) have published QuPPe (Quick Polar Pesticides) methods for the simultaneous analysis of a number of highly polar pesticides which cannot be easily analysed using routine QuEChERS based extraction methods and multi-residue methods (M. Anastassiades et al; QuPPe of EURL-SRM (Version 9.1; 2016). To meet the needs of analysing highly polar pesticides by LC-MS/MS several chromatographic conditions have been used including hydrophilic interaction liquid chromatography (HILIC), zwitterionic-type mixed-mode, normal-phase columns operated in HILIC-mode (bare silica and silica-based chemically bonded columns (cyano and amino)), reversed-phase C18 and carbon based phases. In this work SFC-MS/MS was applied to the analysis of a panel of highly polar pesticides extracted from several food matrices by QuPPe.
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LCMS-8060 Application - Fully automated derivatization - 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. Here we report a fully automated derivatization followed by LC-MS/MS analysis of beer samples. The instrumental set-up does not require any additional hardware for sample pretreatment but uses the built-in pretreatment function of the autosampler.
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LCMS-8060 Application - Applying 'MRM Spectrum Mode' and Library Searching for Enhanced Reporting Confidence in Routine Pesticide Residue Analysis (UK)
To help reduce the incidence of false positive and false negative reporting in pesticide residue monitoring routine multiple-reaction monitoring (MRM) methods have been enhanced to monitor a higher number of fragment ion transitions to increase specificity and reporting confidence. In this workflow, typically 6-10 fragment ion transitions were monitored for each target pesticide as opposed to a conventional approach using 2-3 fragment ions. By acquiring a high number of fragment ion transitions, each target pesticide had a corresponding fragmentation spectra which could be used in routine library searching and compound verification using reference library match scores. This ‘MRM Spectrum Mode’ was applied to quantify and identify 193 pesticides using 1,291 MRM transitions without compromising limits of detection, linearity or repeatability.
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EDX and FTIR Application - Contaminant Analysis Using EDXIR-Analysis Software for Combined EDX-FTIR Analysis
When contaminants are generated, it is important to quickly identify them, ascertain the source, and take measures against further occurrence. Energy dispersive X-ray spectroscopy (EDX) and Fourier transform infrared spectroscopy (FTIR) are very effective techniques for the identification of contaminants. Using EDX and FTIR together provides a simple method of obtaining information on both the elements and compounds present in a contaminant. However, making a comprehensive assessment of sets of EDX and FTIR data to identify a contaminant requires substantial experience and knowledge. EDXIR-Analysis has been recently developed by Shimadzu as software specially designed to identify contaminants to a high degree of accuracy, and contains within it a database of actual contaminant samples and the cumulation of Shimadzu's expertise. In this article, we will describe an example contaminant analysis and in doing so demonstrate the functions and features of EDXIR-Analysis software.
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Prominence Application - Analysis of Melamine and Its Related Substances in Fertilizers
This article describes an example of pretreating and analyzing melamine and its related substances, namely ammeline, ammelide, and cyanuric acid, in fertilizer, in accordance with the testing methods supervised by the Food and Agricultural Materials Inspection Center (FAMIC) in Japan for fertilizers and other substances
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SFC/SFE Application - Online Supercritical Fluid Extraction-Supercritical Fluid Chromatography (Online SFE-SFC)
Online supercritical fluid extraction-supercritical fluid chromatography (online SFE-SFC) system is that directly connects the supercritical fluid extraction (SFE) and supercritical fluid chromatography (SFC). By using the online SFE-SFC, pretreatment to analysis can be automated, creating advantages such as simplification of pretreatment, analysis of unstable compounds, and high-sensitivity analysis. Here, we introduce the basic principle of online SFE-SFC, the characteristics of the “Nexera UC Online SFE-SFC System,” and examples of extraction analyses.
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LCMS-8060 Application - High Sensitivity Analysis of Peanut Allergen in Cumin and Spice Mix (Japan)
Food allergens are a major public health concern. Among them, peanut allergy is one of the common food allergies. To avoid unexpected contact with food allergens, food labels are strictly used to indicate the presence of specific allergens. With the increasing awareness of food allergies, the presence of undeclared peanut in cumin lead to huge recalls in recent years. Although ELISA is the most commonly used technique to detect allergens, its false-positive rate is a major concern due to its cross-reactivity. We developed a method with high specificity and sensitivity to overcome this issue by using a high sensitivity triple quadrupole mass spectrometer to detect peanut allergen Ara h1 in commercially available spices and seasonings.
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LCMS-8060 Application - Ultra-Sensitive and Rapid Assay of Neonicotinoids, Fipronil and Some Metabolites in Honey by UHPLC-LC/MS/MS (Japan)
Neonicotinoids are a class of insecticides widely used to protect fields as well as fruits and vegetables. Recently the use of these 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 European Food Security Authoritiy (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 was necessary. A method was set up using Nexera X2 with LCMS-8060.
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LCMS-8050/8060 Application - Multi-residue analysis of pesticides in crude food extracts using a simple extraction technique and LC/MS/MS
Analysis of pesticide residues in food is typically tedious and time-consuming due to the necessary extraction and clean up procedures. Furthermore, to deal with the ever-growing number of pesticides, the food safety laboratories need to ideally screen as many compounds as possible in a single run which may reach maximum residual limits (MRL); typically 10 ppb in food matrices. In this study, we illustrate the results utilizing an UF MRM capability (just 5 msec. MRM measurement includes dwell and pause time) with 5 msec. polarity switching (UF switching) for the analysis of 146 pesticides in crude food extracts by using easy and simple sample preparation technique.
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LCMS-8050/8060 Application - Shimadzu Pesticide MRM Library Support for LCMSMS
To help expand capabilities in LC/MS/MS pesticide monitoring programs we have created the Shimadzu Pesticide MRM Library. The Library has been created with 766 certified reference standards and has been verified for use with Shimadzu LCMS-8050 and 8060 systems.
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LCMS-8060 Application - Multi-Residue Analysis of 18 Regulated Mycotoxins by LC/MS/MS (UK)
Mycotoxins are one of the most important contaminants in food and feed due to their widespread distribution in the environment and toxic effects on humans and animals. Structurally, mycotoxins are a very diverse group with a wide range of physicochemical properties and low molecular weights. They are produced by fungi (mould) frequently found on agricultural produce, and are often not visible to the naked eye. Some of the most commonly contaminated food stuffs include wheat, oats, rye, corn, barley, rice, nuts and milk. Due to the risks posed by mycotoxins in food they are regulated globally, including, the EU, US, China, Singapore and Brazil. In the EU, reporting limits are harmonised in Regulation (EC) No 1886/2006 (amended by (EC) No 1126/2007) and sampling and analysis in Regulation (EC) No 401/2006. LC/MS/MS is the technique most commonly employed for mycotoxin quantitation in order to achieve the necessary low reporting limits in complex food and feed matrices.
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LCMS-8060 Application - High Sensitivity Analysis of Pesticides in Dried Hops Cones and Hops Pellets by Liquid Chromatography- Triple Quadrupole Mass Spectrometery (SSI)
Hops (Humulus lupulus) are an essential ingredient in brewing beer but agricultural production of this plant is threatened by insects and other dangers. Pesticides and other chemicals may be used to protect hops and increase yield, but certain chemical residues may be harmful to consumers. Chemical residues may also have unintended negative effects on non-target insects such as honeybees. Sensitive and selective detection of chemical residues in hops is necessary to ensure protection of consumers and the environment. Methods using LC-MS provide efficient and effective detection of chemical residues in a complex sample matrix such as hops. We have developed an LC-MS method for detection of over 150 analytes in hops and carried out a market survey of over 50 different hops pellets samples.
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