A chromatography method for the screening and confirmatory detection of dexamethasone

Corticosteroids, such as dexamethasone, have been illegally used as growth promoting agents to obtain an economical benefit from increased muscle development. These substances remain in meat and other animal products and may have negative toxic consequences for consumers. A screening and confirmatory method for dexamethasone detection in feed and drinking water in livestock has been developed and validated. This method is based on immunoaffinity chromatography followed by reverse-phase high-performance liquid chromatrography (IAC–HPLC) with diode array detection (DAD) at 242 nm. Flumethasone was used as internal standard.

The method has been validated according to the European Union regulation 2002/657/EC for banned substances and, thus, the specificity, decision limit, detection capability, recovery and repeatability have been determined. The decision limits (CC) were 26 ng/mL for water and 190 ng/g for feed while detection capabilities (CCβ) were 30 ng/mL for water and 217 ng/g for feed. The method showed good accuracy and precision. The stability of dexamethasone under frozen storage has been studied over a 3.5-month period. No losses were observed, thus confirming that water samples taken by inspectors can be stored frozen for a few weeks until analysis. This method has proved to be relatively simple and useful for rapid screening and confirmation of the presence of dexamethasone in water and feed used for meat-producing animals.     

动物源食品基质中性激素多残留分析方法研究进展

食用动物饲养中促生长性激素的滥用已经成为全球性的食品安全问题,因为这类性激素残留于食品基质中通过食物链被人体摄入后,会对人体造成极大的危害。食品分析领域的研究者长期致力于研究开发食品中性激素多残留的快速、可靠、低成本的检测方法。本文对近年来食品基质中性激素多组分残留分析方法的发展,以及前处理方法（提取与净化）进行了概述,旨在为食品基质中性激素多残留检测及检测方法研究者提供有益的参考。文章首先对性激素作简要介绍,然后对性激素的分析方法包括提取和净化技术进行概述。引用文献47篇。     

高效液相色谱-串联质谱法测定动物源性基质中 氟喹诺酮及四环素类抗生素残留

目的建立高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry,HPLC-MS/MS)检测动物源性基质中的氟喹诺酮和四环素类抗生素残留。方法样品经EDTA-Mcllvaine缓冲溶液提取,超低温冷冻离心脱脂,过亲水亲油平衡(hydrophile lipophile balance,HLB)净化柱,采用Agilent C18柱(100 mm×2.1 mm,2.7μm),以0.1%甲酸-甲醇为流动相,用多离子反应监测(multiple reaction monitoring,MRM)模式进行质谱检测,基质曲线外标法定量。结果该方法对以上13种抗生素类化合物的线性范围为0.02~20μg/kg,相关系数(R)大于0.9923;氟喹诺酮类抗生素的检出限为0.01~0.15μg/kg,定量限为0.03~0.40μg/kg,四环素抗生素的检出限为0.08~0.15μg/kg,定量限为0.27~0.40μg/kg。在0.4、2.0、10μg/kg 3个添加水平的回收率为84.1%~105.0%,相对标准偏差为1.15%~7.81%。结论该方法简单、快速、干扰小,适合动物源性基质体系中兽药残留检测。     

深圳市市售动物源性食品中氯霉素残留量暴露评估

目的 调查研究深圳市市售动物源性食品中氯霉素残留状况及暴露风险,为引导消费和开展安全监管提供借鉴和参考。方法 随机采集2018—2019年深圳市市售畜肉、禽肉、水产品共计511份,使用超高效液相色谱-串联质谱法测定样品中氯霉素的含量,采用点评估法计算深圳市居民通过食用动物源性食品的氯霉素暴露量,并采用暴露边界比(MOE)法对其健康风险进行评估。结果 160份畜肉和60份禽肉中未检出氯霉素,291份水产品(包括贝类、虾、淡水鱼)中氯霉素检出率为26.80%(78/291),其中贝类样品中氯霉素含量为0.05～205.00μg/kg,平均值为13.71μg/kg,检出率为37.21%(64/172);虾样品中氯霉素含量为0.05～2.20μg/kg,平均值为0.20μg/kg,检出率为13.64%(3/22);淡水鱼样品中氯霉素含量为0.05～1.90μg/kg,平均值为0.11μg/kg,检出率为11.34%(11/97),所有样品中氯霉素总检出率为15.26%(78/511)。膳食暴露风险评估结果表明,深圳市居民膳食动物源性食品摄入氯霉素的平均日暴露量为2.06×10^-3     

超高效液相色谱-串联质谱法同时检测动物源性食品中残留的35种β-受体激动剂和11种β-受体阻断剂

针对动物肌肉、肝脏等动物源性食品建立了一种超高效液相色谱-串联质谱法同时检测动物源性食品中残留的35种β-受体激动剂和11种β-受体阻断剂残留量的方法。通过优化萃取溶剂、净化条件、样品基质效应的消除、色谱-质谱条件等参数,提高检测方法的灵敏度和适用性。并且对定量检测方法阿德灵敏度、准确度、精密度等指标进行了验证。结果表明:46种化合物在0.05μg/kg^10μg/kg的空白添加浓度范围内呈良好的线性关系,平均回收率为62.31~110.52%,相对标准偏差为1.03~13.33%。该方法快速、灵敏、准确,稳定,适用于食品安全突发事件的快速应急处置工作。