[Simultaneous determination of beauvericin and four enniatins in eggs by ultra-performance liquid chromatography-tandem mass spectrometry coupled with cold-induced liquid-liquid extraction and dispersive solid phase extraction]. 2021

Bolin Liu, and Man Ni, and Xiaomei Shan, and Ji'an Xie, and Yanyu Dai, and Cheng Zhang
Anhui Provincial Center for Disease Control and Prevention, Hefei 230601, China.

Enniatins (ENNs) and beauvericin (BEA), known as emerging mycotoxins, are the toxic secondary metabolites produced by various Fusarium species. Most grain and grain-based products are contaminated with ENNs and BEA. Animals have been exposed to ENNs and BEA primarily due to consumption of cereal grains and cereal by-products. ENNs and BEA have been detected in animal-derived food and human breast milk, and they pose significant threats to public health. Therefore, more contamination data are urgently needed for the risk assessment of ENNs and BEA present in animal-derived food. To ensure the quality of animal-derived food, a method has been developed for the simultaneous detection of five emerging mycotoxins (viz. enniatin B, enniatin B1, enniatin A, enniatin A1, and beauvericin) in eggs by ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) coupled with cold-induced liquid-liquid extraction (CI-LLE) and dispersive solid phase extraction (DSPE). The main factors governing the response, recovery, and sensitivity of the method, such as the type of extraction solvent, the temperature and duration of cold treatment in CI-LLE, the type and dosages of adsorbents, and apparatus conditions and the type of mobile phase used, were optimized during sample pretreatment and instrument analysis. The mycotoxin residues in eggs were extracted using 20 mL acetonitrile-water-acetic acid (79∶20∶1, v/v/v) mixture for 20 min by the vortex shock method. After mixing, the mixture was frozen for 30 min in a freezer at -40 ℃ and centrifuged for 10 min at 10000 r/min. A 2 mL aliquot of the upper acetonitrile layer was purified by using 70 mg of C18 adsorbents. After whirling, the mixtures were centrifuged at 10000 r/min for 5 min. The purified solution was then concentrated to nearly dry in nitrogen atmosphere at 40 ℃. The residues were dissolved in 1.0 mL 80%(v/v) acetonitrile aqueous solution. The target analytes were separated on an ACQUITY UPLC BEH C18 chromatographic column (100 mm×2.1 mm, 1.7 μm) at a column temperature of 40 ℃, with a flow rate of 0.3 mL/min. The injection volume was 5 μL, and gradient elution was conducted using acetonitrile and 5 mmol/L ammonium formate solution as the mobile phases. Multiple reactions monitoring (MRM) was conducted in the positive electrospray ionization (ESI +) mode. The isotope internal standard method was used for quantification of BEA, and the matrix-matched external standard method was used for quantification of four ENNs. The results of the optimized method showed that the five analytes were completely separated by using the above-mentioned chromatographic column. Good linear relationships were obtained for the five mycotoxins in the concentration range of 0.1-50.0 μg/L; the correlation coefficient (r2) ranged from 0.9983 to 0.9997. The limits of detection (LODs) ranged from 0.05 to 0.15 μg/kg, while the limits of quantification (LOQs) ranged from 0.20 to 0.50 μg/kg. Accuracy and precision experiments were conducted by spiking egg samples with known amounts of analytes at three concentration levels (0.5, 5.0, and 25.0 μg/kg, in compliance with the current legislation) with six replicates. The average recoveries of the five analytes ranged from 81.1% to 106%, and the relative standard deviations (RSDs) were between 0.27% and 9.79%. The matrix effects of the analytes were between 2.70% and 45.1% in egg samples after pretreatment by CI-LLE coupled with DSPE. The developed method was applied to the determination of five mycotoxins in rural eggs and commercial eggs. BEA was detected in most rural egg samples, with detection rates of 30.4%. None of the four ENN residues were detected. Therefore, we can conclude that the method described herein has the advantages of sensitivity, stabilization, accuracy, good recovery, and easy operation, and is suitable for the simultaneous and rapid determination of BEA and ENN residues in eggs.

UI MeSH Term Description Entries
D002851 Chromatography, High Pressure Liquid Liquid chromatographic techniques which feature high inlet pressures, high sensitivity, and high speed. Chromatography, High Performance Liquid,Chromatography, High Speed Liquid,Chromatography, Liquid, High Pressure,HPLC,High Performance Liquid Chromatography,High-Performance Liquid Chromatography,UPLC,Ultra Performance Liquid Chromatography,Chromatography, High-Performance Liquid,High-Performance Liquid Chromatographies,Liquid Chromatography, High-Performance
D004531 Eggs Animal reproductive bodies, or the contents thereof, used as food. The concept is differentiated from OVUM, the anatomic or physiologic entity.
D005506 Food Contamination The presence in food of harmful, unpalatable, or otherwise objectionable foreign substances, e.g. chemicals, microorganisms or diluents, before, during, or after processing or storage. Food Adulteration,Adulteration, Food,Adulterations, Food,Contamination, Food,Contaminations, Food,Food Adulterations,Food Contaminations
D000818 Animals Unicellular or multicellular, heterotrophic organisms, that have sensation and the power of voluntary movement. Under the older five kingdom paradigm, Animalia was one of the kingdoms. Under the modern three domain model, Animalia represents one of the many groups in the domain EUKARYOTA. Animal,Metazoa,Animalia
D047630 Depsipeptides Compounds consisting of chains of AMINO ACIDS alternating with CARBOXYLIC ACIDS via ester and amide linkages. They are commonly cyclized. Cyclic Depsipeptide,Cyclodepsipeptide,Depsipeptide,Peptolide,Peptolides,Cryptophycins,Cyclodepsipeptides,Depsipeptides, Cyclic,Cyclic Depsipeptides,Depsipeptide, Cyclic
D052616 Solid Phase Extraction An extraction method that separates analytes using a solid phase and a liquid phase. It is used for preparative sample cleanup before analysis by CHROMATOGRAPHY and other analytical methods. Extraction, Solid Phase,Extractions, Solid Phase,Solid Phase Extractions
D053719 Tandem Mass Spectrometry A mass spectrometry technique using two (MS/MS) or more mass analyzers. With two in tandem, the precursor ions are mass-selected by a first mass analyzer, and focused into a collision region where they are then fragmented into product ions which are then characterized by a second mass analyzer. A variety of techniques are used to separate the compounds, ionize them, and introduce them to the first mass analyzer. For example, for in GC-MS/MS, GAS CHROMATOGRAPHY-MASS SPECTROMETRY is involved in separating relatively small compounds by GAS CHROMATOGRAPHY prior to injecting them into an ionization chamber for the mass selection. Mass Spectrometry-Mass Spectrometry,Mass Spectrometry Mass Spectrometry,Mass Spectrometry, Tandem
D059625 Liquid-Liquid Extraction The removal of a soluble component from a liquid mixture by contact with a second liquid, immiscible with the carrier liquid, in which the component is preferentially soluble. (McGraw-Hill Dictionary of Scientific and Technical Terms, 6th ed) Liquid Phase Extraction,Extraction, Liquid Phase,Extraction, Liquid-Liquid,Extractions, Liquid Phase,Extractions, Liquid-Liquid,Liquid Liquid Extraction,Liquid Phase Extractions,Liquid-Liquid Extractions,Phase Extraction, Liquid,Phase Extractions, Liquid

Related Publications

Bolin Liu, and Man Ni, and Xiaomei Shan, and Ji'an Xie, and Yanyu Dai, and Cheng Zhang
December 2017, Se pu = Chinese journal of chromatography,
Bolin Liu, and Man Ni, and Xiaomei Shan, and Ji'an Xie, and Yanyu Dai, and Cheng Zhang
September 2013, Se pu = Chinese journal of chromatography,
Bolin Liu, and Man Ni, and Xiaomei Shan, and Ji'an Xie, and Yanyu Dai, and Cheng Zhang
July 2019, Journal of separation science,
Bolin Liu, and Man Ni, and Xiaomei Shan, and Ji'an Xie, and Yanyu Dai, and Cheng Zhang
July 2014, Se pu = Chinese journal of chromatography,
Bolin Liu, and Man Ni, and Xiaomei Shan, and Ji'an Xie, and Yanyu Dai, and Cheng Zhang
December 2020, Se pu = Chinese journal of chromatography,
Bolin Liu, and Man Ni, and Xiaomei Shan, and Ji'an Xie, and Yanyu Dai, and Cheng Zhang
March 2020, Wei sheng yan jiu = Journal of hygiene research,
Bolin Liu, and Man Ni, and Xiaomei Shan, and Ji'an Xie, and Yanyu Dai, and Cheng Zhang
November 2014, Se pu = Chinese journal of chromatography,
Bolin Liu, and Man Ni, and Xiaomei Shan, and Ji'an Xie, and Yanyu Dai, and Cheng Zhang
September 2023, Wei sheng yan jiu = Journal of hygiene research,
Bolin Liu, and Man Ni, and Xiaomei Shan, and Ji'an Xie, and Yanyu Dai, and Cheng Zhang
January 2021, Wei sheng yan jiu = Journal of hygiene research,
Copied contents to your clipboard!