A method and system for separating and determining the residual quantity of four imidazole enantiomers in milk by using ultra-high performance liquid chromatography

By combining ultra-high performance phase chromatography with specific pretreatment and chiral chromatographic columns, the problem of separating tetraimidazole enantiomers in milk has been solved, enabling rapid and accurate enantiomer detection, improving detection efficiency and sensitivity, and making it suitable for quality control and risk assessment of dairy products.

CN122409903APending Publication Date: 2026-07-17HANGZHOU CUSTOMS TECHNICAL CENTER +1
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
HANGZHOU CUSTOMS TECHNICAL CENTER
Filing Date
2026-05-12
Publication Date
2026-07-17

AI Technical Summary

Technical Problem

Existing technologies are difficult to rapidly and accurately separate and quantify the two enantiomers of tetraimidazole in milk, and are easily interfered with by impurities such as proteins and fats under complex matrix conditions, resulting in insufficient detection sensitivity and separation efficiency.

Method used

Ultra-high performance phase chromatography (UHPLC) combined with alkalization-salting-out ethyl acetate extraction and MCX solid-phase extraction purification was employed. An Acquity Trefoil CEL2 chiral column, supercritical carbon dioxide mobile phase, and 0.5% (v/v) ammonia-methanol solution modifier were used to achieve rapid and stable separation of tetraimidazole enantiomers, which were then quantified using a diode array detector.

Benefits of technology

It achieves efficient baseline separation, low matrix interference, high recovery rate and high sensitivity detection of tetraimidazole enantiomers in milk matrix, supporting accurate monitoring and risk assessment of tetraimidazole enantiomer residues in dairy products.

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Abstract

The application relates to the technical field of pesticide residue detection, in particular to a method and system for separating and determining the residue amount of tetramisole enantiomers in milk by using ultra-high performance liquid chromatography. The method comprises the following steps: after alkali treatment and salting-out, a milk sample is extracted by using ethyl acetate, the extracted solution is acidified and redissolved, then purified through an MCX solid-phase extraction column, the eluent is blown dry, and then constant volume is performed by using acetonitrile; an Acquity Trefoil CEL2 chiral chromatographic column is used, carbon dioxide is used as a main mobile phase, 0.5% (v / v) ammonia methanol solution is used as a modifier, gradient elution separation is performed under the conditions of 13.8 MPa system back pressure and 40 DEG C column temperature, and PDA detection is performed, and external standard quantification is performed. The method can realize rapid baseline separation of (+) tetramisole and (-) tetramisole in milk, has the advantages of high sensitivity, high recovery rate, good repeatability and small matrix interference, and is suitable for the detection and supervision of tetramisole enantiomer residues in dairy products.
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