Food Chemistry-X
·
2024
·
IF 6.5
Yan Yang,Xin Li,Jian Lin,Rong Bao
Antibiotics and sedatives are used in freshwater fish culture and transportation, and residue in freshwater fish pose potential risks to human health. Therefore, a throughput method was developed to detect antibiotic and sedative residues in fish, simultaneously quantifying 68 antibiotics and 9 sedatives in freshwater fish using a modified QuEChERS extraction method and UPLC-MS/MS. Matrix-matched calibrations demonstrated good correlation coefficients (R 2 > 0.995), with a recovery range of 66.2–118.5%. The intra-day and inter-day relative standard deviation (RSD) were below 9.7% and 12.8%, respectively. The limits of detection (LOD) and quantification (LOQ) were 0.08–1.46 μg/kg and 0.25–4.86 μg/kg, respectively. 68.8% of analytes had weak matrix effects, and 13.0% had moderate matrix effects. In addition, diazepam and many types of antibiotics were detected in30 freshwater fish. The validation parameters were in agreement with the acceptable criteria of the Codex guidelines. The method was effective in analyzing antibiotic and sedative residues in freshwater fish.
研究领域:
食品安全
·
分析化学
·
环境科学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
FOOD CHEMISTRY
·
2022
·
IF 9.231
Qin Huang,Hua Zhou,Xianglun Wu,Chenli Song,Jiangang Zheng,Meikang Lei,Pengqian Mu,Pinggu Wu
Liquid chromatography coupled with quadrupole linear ion trap tandem mass spectrometry (LC-QLIT-MS/MS) technology operated in electrospray ionization (ESI) was developed for tracing anesthetic (AETs) and sedatives (SDTs) in fish. Sampling procedure was achieved by using acetonitrile extraction followed by dispersive solid phase extraction (DSPE) clean-up. Under the optimized laboratory conditions, reliable qualitative confirmation was obtained through the multiple reaction monitoring-information dependent acquisition-enhanced product ion (MRM-IDA- EPI ) mode. Results indicated a favorable linear in the concentration range of 1–100 μg∙kg −1 (0.1–10 μg∙kg −1 for MS-222), with regression coefficient not less than 0.9997. The detection limit ranges from 0.03 to 0.4 μg∙kg −1 (S/N = 3). The validated method was applied to determine AETs and SDTs in fish with satidfied recoveries of 86.3 %–111.7 % and the relative standard deviations (RSD) of 1.9 %–8.9 % (n = 6). Practical samples analysis indicated that the proposed method is simple, rapid, sensitive and accurate for identification of AETs and SDTs.
研究领域:
分析化学
·
食品安全
✓ 已验证
产品关联
DOI
PubMed
高影响因子
RAPID COMMUNICATIONS IN MASS SPECTROMETRY
·
2020
·Vol. 34
·期 10
·e8742
·
IF 2.2
Jichao Liu,Guoliang Li,Di Wu,Yanxin Yu,Jian Chen,Yongning Wu
Rationale Sedatives, which are prone to cause residues in animals, have been abused in modern animal husbandry. Long-term consumption of contaminated meat products would be unfavorable to the human nervous system. Taking into account public health and food safety, it was essential to develop an effective method for the enrichment and detection of sedatives in meat. Methods Fe 3 O 4 @TbBd@ZIF-8 composites were synthesized by using Fe 3 O 4 nanoparticles as a magnetic core and 1,3,5-triformylbenzene (Tb) and benzidine (Bd) as two building blocks to form Fe 3 O 4 @TbBd. Furthermore, the zeolitic imidazolate framework-8 (ZIF-8) was modified on the surface of the Fe 3 O 4 @TbBd. In addition, Fe 3 O 4 @TbBd@ZIF-8 was used as a magnetic solid-phase extraction (MSPE) adsorbent of typical animal sedatives in pork samples. Mass spectrometry analysis was conducted by electrospray ionization triple-quadrupole mass spectrometry in positive-ion multiple reaction monitoring mode. Results By combining the optimized MSPE approach with high-performance liquid chromatography/tandem mass spectrometry (HPLC/MS/MS), an accurate and sensitive method for the determination of sedatives was developed. The method exhibited good linearity in the range of 0.03–70 μg/kg with the correlation coefficient (R 2 ) ranging from 0.9982 to 0.9999, high sensitivity with limits of detection (LODs) ranging from 0.04 to 0.2 μg/kg, and high precision with relative standard deviation (RSD) less than 5.5%. The adsorption behaviors of Fe 3 O 4 @TbBd@ZIF-8 towards sedatives were more suitably described by a pseudo-second-order kinetic and Freundlich isotherm model. Conclusions The proposed MSPE-HPLC/MS/MS method was successfully applied to the determination of sedatives in real samples and showed excellent applicability. Several sedatives were detected in the selected meat samples. The developed method was shown to be facile, sensitive and accurate for sedative detection and also showed great prospects for determination of sedatives from other complex samples.
研究领域:
分析化学
·
食品安全
·
材料科学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
ANALYTICAL SCIENCES
·
2023
·Vol. 39
·期 12
·1939-1946
·
IF 1.6
Xiang Jian Jun,Yuan Li Juan,Liao Qie Gen,Zhang Da Wen,Luo Lin Guang
Azo-linked covalent organic polymers (ACOPs) were synthesized by a simple azo reaction, with 2,2ʹ-bis(trifluoromethyl)benzidine and 1,3,5-trihydroxybenzene as the monomers. The preparation process was mild, green, and environmental-friendly, avoiding the use of high temperature, metal catalysis, and harmful organic reagent. The obtained ACOPs were characterized by scanning electron microscopy, Fourier transform infrared spectroscopy, thermogravimetric analysis, powder X-ray diffraction, and Brunauer–Emmett–Teller. With the prepared ACOPs as adsorbent, a method of pipette tip solid-phase extraction–liquid chromatography–tandem mass spectrometry detection (PTSPE–LC–MS/MS) was proposed for the analysis of target sedatives in animal tissues. Furthermore, the parameters for the extraction of five sedatives, including the amount of adsorbent, pH value, ion strength, elution solvent and volume, were investigated. Under the optimized conditions, the linear dynamic range was found from 0.1 to 10.0 μg kg −1 , and the limits of detection were ranged from 0.02 to 0.1 μg kg −1 . The method was assessed by the analysis of target sedatives in animal tissues, and the recoveries for the spiked pork muscle and pork liver samples were 84–102% and 83–101%, respectively. The results show that the developed method of PTSPE–LC–MS/MS with ACOPs as adsorbent is efficient for the analysis of trace sedatives in animal tissues. Graphical Abstract
研究领域:
分析化学
·
食品安全
✓ 已验证
产品关联
DOI
PubMed
高影响因子
危险品化学品经营许可证（带存储）