Abstract

This paper described an organic solvent-free, rapid, simple, and space-saving method of sample preparation followed by HPLC coupled photo-diode array (PDA) detector for simultaneous quantification of cyromazine (CYR) and its decycropropylated metabolite, melamine (MEL), in milk. The HPLC-PDA was performed on an InertsilR HILIC column with an isocratic aqueous mobile phase. Analytes were extracted from the sample using water, and purified by MonoSpinR-C18, a centrifugal monolithic silica spin mini-columns, and quantified within 20 min. The method, performed under 100% aqueous conditions, obtained average recoveries for CYR and MEL in the range of 93.2 . 99.1% with relative standard deviations . 2.8%. The quantitation limits were 8.5 ng/mL for CYR and 10 ng/mL for MEL, respectively. No organic solvents were used at any stage of the analysis.

Highlights

  • Cyromazine (CYR) is a triazine insect growth regulator used as an insecticide

  • The Food Safety and Inspection Service (FSIS) of the United States Department of Agriculture (USDA) have been provided a test method based on high-performance liquid chromatography (HPLC) for analyzing CYR and MEL in animal tissues in its Chemistry Laboratory Guidebook which contains test methods used by FSIS Laboratories to support the Agency’s inspection program, ensuring that meat, poultry, and egg products are safe, wholesome and accurately labeled [10]

  • Previous techniques based on high-performance liquid chromatography (HPLC) for simultaneous determination of CYR and MEL in animal-derived foods [11,12,13,14,15] has crucial drawbacks: 1) all of methods consume organic solvents in the instrumental analyses as well as for extraction and de-proteinization in sample preparation

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Summary

Introduction

Cyromazine (CYR) is a triazine insect growth regulator used as an insecticide. In veterinary medicine, CYR is used as an ectoparasiticide and is added to animal feed to prevent fly from the manure, so as to improve the hygiene control of animal housing environments. The Food Safety and Inspection Service (FSIS) of the United States Department of Agriculture (USDA) have been provided a test method based on high-performance liquid chromatography (HPLC) for analyzing CYR and MEL in animal tissues in its Chemistry Laboratory Guidebook which contains test methods used by FSIS Laboratories to support the Agency’s inspection program, ensuring that meat, poultry, and egg products are safe, wholesome and accurately labeled [10]. Previous techniques based on high-performance liquid chromatography (HPLC) for simultaneous determination of CYR and MEL in animal-derived foods [11,12,13,14,15] has crucial drawbacks: 1) all of methods consume organic solvents in the instrumental analyses as well as for extraction and de-proteinization in sample preparation. This article describes an ultra safe, idiot proof, and inexpensive method to strictly monitor CYR and MEL residues in milk using a 100% aqueous solution in sample preparation and HPLC separation without organic solvent consumption.

Method validation
Results and Discussion
Conclusion

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