High performance liquid chromatography-fluorescence detection method for 3-chloro-1,2-propylene glycol

Abstract

The invention discloses a high performance liquid chromatography-fluorescence detection method for 3-MCPD. The method comprises the following steps: (1) treating a 3-MCPD aqueous solution, and cracking the 3-MCPD into chloroacetaldehyde; (2) removing excessive periodate, and eliminating side reaction; (3) carrying out fluorescence derivation reaction, namely enabling the chloroacetaldehyde to react with a fluorescence derivation reagent so as to generate a target material with a fluorescence effect; and (4) performing HPLC-FLD measurement, namely separating the target material, and quantifying the 3-MCPD according to the chromatographic peak area, wherein the fluorescence derivation reagent refers to an o-amino binary N-heterocyclic compound. According to the method disclosed by the invention, a type of novel fluorescence derivation reagents with convenient and readily available materials, high selectivity, high fluorescence efficiency and high hydrophobicity can be used for high performance liquid chromatography-fluorescence detection of 3-MCPD, so that the target product has a good retention behavior in the reversed phase liquid chromatography, and the accuracy and sensitivity of the test method are improved.

Description

technical field [0001] The invention relates to a high performance liquid chromatography-fluorescence detection method for 3-chloro-1,2-propanediol, belonging to the field of analytical chemistry. Background technique [0002] 3-Chloro-1,2-propanediol is also known as 3-chloropropanediol or chloroglycerin, its English name is 3-monochloro-1,2-propanediol, abbreviated as 3-MCPD, and its chemical structural formula is: CH 2 Cl-CHOH-CH 2 Oh. 3-MCPD is a kind of monochlorodihydric alcohol, which is a colorless liquid with a sweet taste, freezing point -40°C, boiling point 213°C (decomposition), relative density 1.3218 (20°C), refractive index 1.4809 (20°C), Soluble in water, ethanol, ether and acetone, slightly soluble in toluene, insoluble in benzene, petroleum ether and carbon tetrachloride; unstable, gradually turns rice yellow after standing, easy to absorb moisture. [0003] Toxicity studies in recent years have shown that 3-MCPD has strong hazards to human health and ha...

AI Technical Summary

Problems solved by technology

However, due to the good water solubility and high boiling point of 3-MCPD, the analysis method based on gas chromatography for the determination of 3-MCPD has the disadvantages of complex and cumbersome pretreatment process, harsh derivatization conditions, and high instrument maintenance costs.

In view of this, it is of great significance to develop a low-cost, easy-to-operate high-sensitivity detection method based on high-performance liquid chromatography. Patent CN102565270 first reported a combination of periodic acid oxidative cleavage, base or nucleoside (nucleotide ) derivatized reversed-phase liquid chromatography-fluorescence detection method, which has low test cost, simple operation and high sensitivity, and can be applied to the determination of 3-MCPD in foods such as oils and soy sauces. However, due to the use of fluorescence derivatization The reagent is too hydrophilic, and the retention of the target product in reversed-phase liquid chromatography is weak. When measuring complex food samples, it may be easily interfered by the matrix effect, which affects the accuracy and reproducibility of the measurement. Therefore, the development of new fluorescent properties Good, more hydrophobic fluorescent derivatization reagents will be more conducive to the strengths and advantages of this method

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