An ultrahigh-performance liquid chromatography-tandem mass spectrometry method was developed and validated for the determination of lactoferrin in camel milk based on the signature peptide. The camel lactoferrin was purified by heparin affinity chromatography and then used to screen tryptic signature peptides. The signature peptide was selected on the basis of sequence database search and identified from the tryptic hydrolysates of purified camel lactoferrin by ultrahigh-performance liquid chromatography and quadrupole time-of-flight tandem mass spectrometry. The pretreatment procedures included the addition of isotope-labeled winged peptide and the disposal of lipids and caseins followed by an enzymatic digestion with trypsin. Analytes were separated on an Acquity UPLC BEH 300 C18 column and then detected on a triple-quadrupole mass spectrometer in 7 min. The limits of detection and quantification were 3.8 mg kg−1 and 11 mg kg−1, respectively. The recoveries ranged from 74.5% to 103.6%, with relative standard deviations below 7.7%. The validated method was applied to determine the lactoferrin in ten samples collected from Xinjiang Province.
An ultrahigh-performance liquid chromatography–tandem mass spectrometry method was developed and validated for the simultaneous determination of sterigmatocystin, verruculogen, enniatin A, fusarenon-X, fumonisins B1, B2, B3, aflatoxins B1, B2, G1, G2, ochratoxin A, deoxynivalenol, 3-acetyldeoxynivalenol, 5-acetyldeoxynivalenol, and zearalenone. The mycotoxins were extracted and cleaned up using a multitoxin column, separated on a C18 column, and then detected on a triple-quadrupole mass spectrometer. The limits of detection and quantification ranged within 0.2–2 µg/kg and 1–10 µg/kg, respectively. The recoveries ranged from 70.8 to 118.4%, with relative standard deviations below 15%. The method was used to analyze 80 samples obtained from Shandong Province in China. Fifty-eight samples were contaminated with 10 mycotoxins at concentrations ranging from 1.4 to 6566.1 µg/kg. Some samples exceeded the maximum limits in China and in European regulations for mycotoxins in unprocessed maize.
The study determined 19 elements in peanuts of different regions in China by ICP-MS, and explored a method of identifying peanut origin by multi-element analysis.
3 July 2020 in Food Additives & Contaminants: Part A
In this study, we carried out two experiments to evaluate depletion of florfenicol (FF) and its metabolite florfenicol amine (FFA) in eggs from growing pullets and laying hens. Eggs were collected, and the egg white and yolk were separated. FF and FFA were analysed by liquid chromatography-tandem mass spectrometry. In the first experiment, 30 laying hens were given FF capsules at 50 mg/kg·bw−1 daily for 5 d. FF + FFA was detectable in egg white (1,190 µg/kg) on day 1 of treatment and increased slowly thereafter. After treatment, the residues decreased rapidly and were not detected by day 11. In yolk, residues were detected at a lower concentration on day 1 and increased dramatically to 3308 µg/kg at the end of treatment. The residues remained steady over the next 4 days post-treatment, followed by a rapid drop. Residues were not detectable on day 15 post-treatment. In the second experiment, four groups (B1 through B4) of growing pullets were treated in the same manner for 25, 20, 15, and 10 days before egg primiparity. FF and FFA were not detectable in the eggs of group B1; however, they were detectable in egg whites and yolks of groups B2, B3, and B4. The highest total concentrations of FF and FFA detected in egg white and yolk of group B4 were 3,190 µg/kg and 3,214 µg/kg, respectively. Thereafter, concentrations decreased until no more residues were detected in egg whites or yolks on days 17 and 21 post-treatment, respectively. Therefore, drug treatment should be stopped at least 21 d before primiparity of growing pullets to guarantee food safety.
15 July 2022 in Food Additives & Contaminants: Part A
Some florfenicol (FF) metabolites have a strong binding affinity towards biomolecules in the edible tissues of some food animals. These bound FF residues cannot be extracted directly from edible tissues with organic solvents and are present in higher concentrations even than solvent extractable residues. In this study, an ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was established to detect the total residues of FF in eggs, by quantifying the metabolite florfenicol amine (FFA). The sample was hydrolyzed at 95–100 °C for 4 hours to release sample-matrix bound residues and convert them all into FFA. The hydrolyzed sample was washed with ethyl acetate to remove interfering substances, extracted with ethyl acetate under alkaline conditions, purified by solid phase extraction and quantified by UPLC-MS/MS. The recoveries of FFA in eggs ranged from 91.2 to 102.4%, with an RSD ≤ 10.9%. The LOD and LOQ were 0.5 and 1.0 μg/kg, respectively. This method can be applied to the quantification of total FF residues in eggs.