In this paper, we built a method of verifying the 4 retinols of vitamin A and 8 tocopherol isomers of vitamin E in the food industry based on RP-HPLC-PDA-FLR. The effect of laboratory light conditions on the target components was considered for the first time, and it was found that the loss rate of the target components was the smallest in the case of a white laboratory bench with red or LED light in the dark room. There was no finding of extraction recoveries of the target components with a significant difference under different saponification conditions. Meanwhile, it was found that using ethyl acetate/n-hexane mixed solvent as the extraction solvent could ensure the effective extraction of the target components. Finally, baseline separation of 12 components was achieved within 45 min using the C30 column. With the help of methodological verification, we found that the recovery rate ranged from 76.45% to 93.52%, and RSD was between 0.19% and 12.99%; the Limit of Detection minimum value was 0.01 mg/100 g and the Limit of Quantitation minimum value was 0.03 mg/100 g. The detection method was successfully applied to the distribution detection of 4 kinds of retinols and 8 kinds of vitamin E in egg and dairy products and provided technical support for the accurate nutritional evaluation of vitamin A and vitamin E.
Eggs were used to study the determination and depletion of amoxicillin (AMO) residues after oral dosing hens (25.0 mg kg–1, 50.0 mg kg–1 body weight), once daily for five days. A reverse-phase high-performance liquid chromatography with fluorescence detection (RP-HPLC-FLD) method was developed to determine AMO residues in albumen, yolk and whole egg. By using pre-column derivatisation, an improved liquid–liquid extraction procedure was developed for sample preparation. AMO were extracted from eggs with acetonitrile. The extract solution was extracted using saturated methylene chloride. The supernatant was reacted with salicylaldehyde under acidic and heating conditions. Limits of detection (LODs) were 1.2 ng g–1 and limits of quantification (LOQs) were 3.9 ng g–1 for AMO. Recoveries of AMO from samples fortified at levels of 5.0–125.0 ng g–1 ranged from 79.1% to 88.5% in albumen, 78.6–83.6% in yolk and 78.3–85.1% in whole egg, with coefficients of variation of ≤7.3%. The maximum concentrations of AMO in albumen, yolk and whole egg were found to occur at 1.5, 2.5, 1.5 days after withdrawal of medication respectively. AMO was not detectable in albumen at 7.5 days after final administration of AMO, at 10.5–11.5 days in yolk and 10.5 days in whole egg after administration of two oral doses. The method was applied during the residue study of AMO in order to formulate a reasonable withdrawal period to ensure food safety.
A method was established for the simultaneous trace analysis and identification of 27 sulfonamides and 6 sulfonamide potentiators in eggs by ultrahigh-performance liquid chromatography coupled with quadrupole-high-field orbitrap high-resolution mass spectrometry and multifunction impurity adsorption cleaning. The appropriate extraction, purification, and instrument conditions were optimized. The drugs were extracted by acetonitrile with 1% formic acid and purified with optimized adsorption material based on multifunction impurity adsorption cleaning. The elution was evaporated by nitrogen blowing, dissolved, and then assayed. The limits of detection were 0.01–0.28 μg kg−1 for all drugs, while the recoveries were 82.4–110.6%, the relative standard deviations were 2.5–14.9%, and the linearity of the drugs in the corresponding concentration range was greater than 0.995. The proposed method was successfully applied for the monitoring of sulfonamides and their potentiators in egg samples, whereby 4 sulfonamides and 3 sulfonamide potentiators were detected in 200 egg samples.
As a pretreatment technique to trace analysis, polyoxyethylene lauryl ether (POELE10)- salt aqueous two-phase extraction system (ATPES) is coupled with high performance liquid chromatography to analyse thiamphenicol (TAP) in egg, milk and honey. The analysis of the phase behaviors of the ATPES found that the extraction efficiency and enrichment factor of TAP was influenced by the types of salts, the concentration of salt, the concentration of POELE10, the concentration of 1-propanol and the temperature. The optimized conditions of experiment were determined in the multi-factor experiment by using response surface methodology. The extraction efficiency of TAP is up to 99.59% and the optimal values of enrichment factor of TAP was 27 under the optimized conditions. The limit of detection and the limit of quantification of TAP are 0.5 µg kg−1 and 1.5 µg kg−1, which meet the needs of determination of trace or ultratrace TAP in food.
危险品化学品经营许可证（带存储）