Determination of Veterinary Drug Residues in Animal-derived Foods by Liquid Chromatography-Mass Spectrometry

[Objectives]This study was conducted to establish a rapid and effective method for simultaneous extraction of 54 kinds of veterinary drug residues in animal-derived food, including sulfonamides, quinolones, tetracyclines, malachite greens, penicillins, nitroimidazoles, tranquilizers and macrolides, by HPLC-MS. [Methods] The samples were extracted with 80% acetonitrile water(containing 0.1% formic acid), combined with QuEChERS extraction technology and C18 and PSA purification, analyzed by high performance liquid chromatography-mass spectrometry, and quantified by external standard method. The target substances were analyzed on ZORBAX Eclipse C18 chromatographic column using 0.2% formic acid water and 0.2% methanol as mobile phases. The gradient elution mode was used for chromatographic separation and multiple reaction detection. [Results] In the linear range of 0.5-50.0 ng/ml, the linear relationship of the 54 kinds of veterinary drug residues was good, with correlation coefficients(r~2) greater than 0.995, and the detection limits ranged from 0.30 to 1.00 μg/kg. The results showed that the recovery ranged from 75.4% to 118.2% when different matrixes were added for recovery. [Conclusions] This method is simple, efficient, accurate, stable, and highly operable. It is applicable to simultaneous batch screening of veterinary drug residues in animal-derived food, and has high practical application value.

Research Progress on Analysis and Detection Techniques of Veterinary Drug Residues in Animal Foods

As an important guarantee for the prevention and control of animal diseases,veterinary drugs have important functions in improving animal production performance and product quality and maintaining ecological balance.They are an important guarantee for the healthy development of animal husbandry,food safety and public health.However,the irrational use and abuse of veterinary drugs and feed pharmaceutical additives are widespread,causing harmful substances in animal foods and damage to human health,and threatening the sustainable development of the environment and animal husbandry as well.In order to ensure human health,it is urgent to develop a simple,rapid,high-sensitivity,high-throughput and low-cost veterinary drug residue detection technology.In this paper,the sample pretreatment methods and detection techniques for the analysis of veterinary drug residues in animal foods were reviewed.

Situations and Countermeasures on Veterinary drug residues and Detection to Animal Material Food of Entry-Exit Trade

With the people's lives improving,the demands of livestock products on the import and export aspects were growing. Veterinary drug residues as the important factor which might influence animal products safety has become a major concern. In this paper,the status quo and inspection of the veterinary drug residue and the corresponding control measures were put forward.

Application of Liquid Chromatography-Tandem Mass Spectrometry in Determination of Veterinary Drug Residues

With the long -term and irrational use of veterinary drugs and drug additives in the process of animal feeding, the veterinary drug resi- dues in animals and their additives can be ingested into the human body and pose potential threat to human health. Detection of veterinary drug resi- dues are extremely important practical significance to protect the ecological environment and human health. In recent years, liquid chromatography -tandem mass spectrometry has been widely used in vetednary drug residue detection because of its applicability, qualitative and quantitative fea- tures as well as high sensitivity. This article summarized the application of liquid chromatography -tandem mass spectrometry in detection veterinary drug residues from feed, animal products, arid udne as well as illicit drugs and harmful additives.

Advance in Effect of Veterinary Drug Residues on Ecological Environment

Thousands of tons of pharmaceutically active substances are used in veterinary medicines in intensive livestock and poultry production, but most of the drugs are poorly absorbed by animals and excreted with the animal feces. The veterinary medicines can cause various kinds of harmful impact to the environment. Now the relevant research has been a hot all over the world. With the feces excreted to the environment, the veterinary medicines can be accumulated in the soil and water, and produce all sorts of reaction. Some medicines can cause toxic effect to animals, plants and microorganisms. The article summarized the residue, the environmental impact, the transformation and the development direction of the veterinary medicine in the environment to supply frame of reference for further research.

Application of Liquid Chromatography-High Resolution Time-of-flight Mass Spectrometry in the Detection of Raw Milk and Dairy Products

Milk and dairy products are more and more popular with consumers due to their various nutrients, and their quality and safety issues have always been concerned. Therefore, the development of rapid, accurate and simple screening techniques is of great significance. Liquid chromatography-high resolution time-of-flight mass spectrometry has high-resolution and high-throughput detection functions, and has gradually begun to be applied in the detection of milk and dairy products. This paper summarized the application of milk and dairy products in liquid chromatography-high resolution time-of-flight mass spectrometry, laying a foundation for the development of new methods.

重庆市部分区县鸡肉和鸡蛋兽药残留监测分析及膳食暴露风险评估

目的:了解重庆市部分地区鸡肉和鸡蛋食品中15种兽药残留情况,并评估人体摄入健康风险。方法:2021—2023年,在重庆市17个区县的商场超市、农贸市场随机抽取鸡肉、鸡蛋样品共计107份,采用液相色谱-质谱/质谱法测定鸡肉及鸡蛋中6种喹诺酮类、2种四环素族类、1种硝基咪唑类、2种酰胺醇类抗生素及4种抗球虫药含量。根据重庆市居民的饮食消费情况,采用点评估法和食品安全指数法对鸡肉和鸡蛋中兽药的暴露风险进行评估。结果:76份鸡蛋样品兽药残留检出率为25.00%(19/76),不合格率为2.63%(2/76);鸡肉样品兽药残留检出率为70.97%(22/31),不合格率为0%(0/31);鸡蛋及鸡肉中检出率较高的多西环素,食品安全指数均值分别为0.000 293和0.000 119,最大值分别为0.002 710和0.001 770,均远低于1。结论:重庆市部分区县鸡肉及鸡蛋中兽药残留有不同程度的检出,部分样品不合格,但总体风险较低,健康危害在可接受范围。

固相萃取-液相色谱-串联质谱法测定海参中62种兽药残留

目的建立固相萃取结合高效液相色谱-串联质谱同时测定海参中62种药物的检测方法。方法样品加水分散后经1.0%甲酸乙腈溶液提取,PEP固相萃取柱净化后,采用WatersX-Bridge-C18色谱柱分离、0.2%甲酸水溶液-甲醇为流动相进行梯度洗脱,使用选择离子监测模式检测。结果62种兽药在0.50~100.00ng/m L范围内呈现出良好的线性关系,线性相关系数r^(2)在0.9953~1.0000范围内。方法检出限为0.25~2.50μg/kg;在3个不同浓度添加水平下,62种兽药的平均回收率在70.3%~119.0%,批内和批间的相对标准偏差(n=5)为0.13%~14.90%,均小于15.00%。将该方法应用于30批次海参样品的检测,其中4批次样品的喹诺酮检测结果阳性,检出量为5.30~28.00μg/kg,与国家标准方法的检测结果相比,该方法对于本次喹诺酮药物筛查的准确率为100%。结论该方法灵敏度高,准确度和精密度良好,满足我国兽药残留检测要求,可适用于海参中62种兽药多残留的定性定量分析检测。

我国限制使用的兽药在食品动物中的残留概况

从我国食品动物禁用、停用、特定时期不得使用以及允许使用但不得检出等层面,对我国兽药使用的限制、相关残留检测方法标准适用范围以及相关问题的分析和建议进行综述,以期为养殖业规范用药、食品安全监管部门政策制定和调整、科研机构针对不得检出兽药残留标准相关研究的开展提供参考。

超高效液相色谱-串联质谱法检测畜禽肉中199种药物及代谢物残留

建立了一种可检测猪肉、鸡肉、牛肉和羊肉四种畜禽肉中199种药物及代谢物残留的超高效液相色谱-串联质谱法。样品经Mcllvaine-Na_(2)EDTA缓冲液和2%甲酸乙腈溶液提取后,高速离心去除蛋白质等杂质,用captiva EMR-Lipid小柱净化。以0.1%甲酸乙腈溶液和0.1%甲酸溶液为流动相洗脱,在C_(18)色谱柱上分离。ESI离子源正负离子模式同时扫描,并采用多反应监测模式(MRM)检测,基质匹配标准溶液外标法定量。结果表明:各药物及代谢物在空白猪肉、鸡肉、牛肉和羊肉基质匹配系列浓度范围内均呈现良好的线性关系,相关系数(r)均大于0.990;在4种基质中的定量限范围在0.5~20μg/kg之间;在定量限~200μg/kg添加浓度上的回收率范围为60%~120%,批内与批间相对标准偏差均小于20%。该方法具有简便快捷、选择性好、定性准确,重复性好等特点,可进行多种类药物及代谢物残留的同步处理和同时检测。对提高实际样品检测工作效率,更好的确保动物性食品安全,保护人类健康具有重要意义。

我国蜂产品相关兽药残留法规的变化与现状

随着我国食品中最大兽药残留限量国家标准的颁布更新,对蜂产品的质量安全监管提出了更高要求。本文汇总分析了当今中国蜂蜜主要出口国的蜂产品兽药残留限量标准政策和差异,梳理比较了我国历年发布的相关兽药法规政策,分析了相关兽药政策的变化发展和对蜂产品质量安全的影响。使养蜂者清楚自己可以做什么,监管者了解自己该做什么。这对提高我国蜂产品的质量安全标准和顺畅出口贸易具有重大意义。

不同C_(18)固相萃取柱对鹌鹑蛋中6类兽药残留测定的影响研究

使用不同C_(18)固相萃取柱对鹌鹑蛋进行处理,通过对比基质效应、回收率、精密度的结果,评价不同C_(18)固相萃取柱对6类兽药残留测定情况的影响。结果表明,使用不同C_(18)固相萃取柱后,6类目标物质保留时间出峰一致,且目标物质峰形良好,净化效果基本一致。对同一种化合物的基质效应标准偏差均小于10%。3种不同浓度下,6类兽药的平均回收率为71.4%~116.1%,精密度为2.6%~15.5%,均满足使用效果。

表面增强拉曼光谱在动物源性食品兽药残留检测的研究进展

动物性食品安全问题日益突出,愈演愈烈,有关问题食品的报道也受到了公众的广泛关注。一旦兽药在畜牧养殖过程中被过度使用或滥用,药物残留将给人类健康带来严重危害。常见的残留检测方法存在成本高、速度慢和效率低等缺点,通常需要专业人员操作,传统的理化方法已不能满足食品质量检测的需要,因此研发快速高效的兽药残留检测方法起着关键作用。近年来,表面增强拉曼光谱(SERS)技术在真伪鉴别、非法添加物检测和农兽药残留等诸多领域得到了广泛应用,并以其快速检测、无损等优势在食品检测领域有着更为广阔的发展前景。与其他检测方法不同的是,SERS通过信号放大和高灵敏度的指纹光谱,可以快速识别目标分析物,进行定性或半定量分析。本文主要介绍了拉曼光谱和SERS在动物源性食品中兽药残留检测中的研究和应用,重点介绍了SERS的优势、食品样品的前处理以及SERS结合其他技术检测多种兽药的相关研究,并提出了SERS在实际监测中面临的挑战。

一步净化结合超高液相色谱串联质谱同时测定雅鱼中13类54种兽药残留

目的:本研究建立了一种一步净化法结合液相色谱串联质谱(LC-MS/MS)同时检测雅鱼(Schizothorax prenanti)中13类54种兽药残留的快速检测方法。方法:向2.0 g样品中加入8 mL 0.2%甲酸-乙腈:水溶液(90:10,V/V)提取,冰水浴超声提取,LPAS一步净化。采用C18柱,甲醇-0.1%甲酸/5 mmol/L乙酸铵溶液梯度洗脱,动态多反应监测(dMRM),正/负离子模式,内标法定量,LC-MS/MS测定。以添加54种兽药的方式,对提取方式、提取体积、盐的加入、液相和质谱条件进行了优化,对方法性能(基质效应、方法检出限、方法定量限、准确度、精密度)等进行了验证。结果:54种兽药在0.1~50μg/L范围内线性关系良好,决定系数(R^(2))≥0.992,方法检出限(LOD)为0.03~2.5μg/kg之间,方法定量限(LOQ)为0.1~8.3μg/kg之间,在低(添加量5~10μg/kg)、中(添加量10~20μg/kg)、高(添加量50μg/kg)三个水平下54种药物的平均回收率为70.45%~118.1%,RSD为0.01%~9.9%。对50份养殖雅鱼样本应用该方法进行检测,7份样品有药物检出,恩诺沙星和达氟沙星各检出2次,磺胺甲噁唑检出4次,均低于定量限的定性检出。结论:该方法操作简单,一步净化,且方法检出限低、灵敏度高,准确度和精密度均较好,方法性能验证其符合多种兽药残留要求,可为大批量检测雅鱼中多种类兽药残留提供有力支持。

畜禽产品中兽药残留的危害及防控策略

随着畜禽动物养殖集约化、规模化的发展,畜禽产品的生产量、销售量也逐年增长,畜禽产品中兽药残留问题已成为全社会广泛关注的热点问题。畜禽动物养殖过程中,兽药是重要投入品,主要用来预防、治疗动物疾病。如若兽药使用不合理易造成畜禽产品中兽药残留,会直接影响畜禽产品质量安全和生态健康,进而可能会威胁到消费者的人体健康。基于此,文章综述了兽药残留的危害,兽药残留产生的主要原因以及兽药残留防控策略,为保障畜禽产品质量安全提供技术支持。

量子点免疫层析技术在兽药残留快速检测中的应用

近年来,免疫层析技术在动物源食品的现场快速检测中发挥了重要作用,对开展兽药残留高效监管提供了有力保障。量子点作为新型荧光材料,用作免疫层析检测中的标记材料,能够有效提高检测性能,在快速检测技术研究领域具有广阔的应用前景。文章总结了量子点的分类、合成及免疫探针的制备,综述了量子点免疫层析技术在动物源食品兽药残留快速检测中的应用进展,并对量子点免疫层析检测技术在量子点合成、兽药人工抗原及抗体制备方面的研究进行了展望。

基于金属有机框架材料的农产品中农兽药残留快速检测与去除研究进展

农产品中农兽药残留的检测与去除是食品安全风险防控的重要环节。目前检测农兽药残留的方法主要是仪器分析法,但存在检测时间长、操作要求高等不足,无法满足快速检测的需求。金属有机框架(Metal-Organic Frameworks,MOFs)是一种由金属离子或金属簇与有机配体构成的杂化材料,其具备吸附富集、催化降解、可发荧光及产生电化学信号等功能,因而具有良好的潜力应用于农兽药残留的快速检测与去除。本文阐述了MOFs材料的富集去除、催化降解、荧光传感和电化学传感四种功能,总结了基于MOFs的不同功能开发的农兽药残留快速检测与去除方法,综合分析了结合RGB分析技术与便携式监测设备后的优势与不足,讨论了MOFs应用于农兽药残留检测与去除的挑战。本文为MOFs快速检测技术的进一步发展提供参考。

通过式固相萃取结合高效液相色谱-四极杆飞行时间质谱测定鸡蛋中62种兽药残留

建立了固相萃取结合高效液相色谱-四极杆飞行时间质谱(HPLC-QTOF)同时测定鸡蛋中62种兽药残留的方法。鸡蛋均质后经90%甲酸乙腈水溶液提取后,PRiME HLB固相萃取小柱净化,氮吹后复溶,用(HPLC-QTOF)进行检测。62种兽药在0.5~500 ng/mL浓度范围内线性关系良好(r^(2)≥0.99),回收率在71.2%~113%之间,日内变异系数范围为1.3%~14.3%,日间变异系数范围为4.2%~18.3%,检测限为1.0~2.0μg/kg,定量限为2.0~5.0μg/kg。本方法简便快捷、准确可靠,适用于鸡蛋中62种兽药的同时测定。

QuEChERS结合高效液相色谱串联质谱法检测猪肉中16种兽药残留

建立了一种QuEChERS前处理与高效液相色谱串联质谱法(HPLC-MS/MS)相结合同时检测猪肉中16种兽药残留的方法。样品采用水−0.1%甲酸乙腈经QuEChERS技术提取和净化后,在正离子多反应监测模式(multiple reaction monitoring,MRM)下进行分析测定。结果表明:16种兽药在2.0~100.0μg·kg^(−1)的范围内有良好的线性关系(相关系数r>0.9970);检出限(LOD,S/N=3)和定量限(LOQ,S/N=10)的范围分别为0.01~0.25μg·kg^(−1)、0.03~0.82μg·kg^(−1);在猪肉样品中进行了2、4、20μg·kg^(−1)3个不同浓度水平的加标试验,相对标准偏差RSD为1.1%~9.0%,加标回收率在70.4%~118.1%。该方法的重复性和回收率满足试验要求,灵敏度高,适用于猪肉中多种类兽药残留的分析检测。

内蒙古部分地区鸡蛋中土霉素和强力霉素检测及膳食风险评估

目的了解内蒙古自治区部分地区鸡蛋中土霉素和强力霉素残留情况,并评估膳食风险。方法在内蒙古自治区部分地区的农贸市场、商店、网店等采集共180份样品,采用液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometry,LC-MS/MS)进行检测,分析鸡蛋中的土霉素、强力霉素残留含量,根据内蒙古居民的饮食消费情况,采用点评估法和食品安全指数法对鸡蛋中兽药的暴露风险进行评估。结果2022—2023年内蒙古自治区部分地区土霉素、强力霉素总体样本检出率为24.44%(44/180),超标率为12.22%(22/180)。强力霉素检出42份,检出率为23.33%(42/180),超标率为12.22%(22/180);土霉素检出3份,检出率为1.67%(3/180),此次调查中无超标样本;鸡蛋中强力霉素食品安全指数均值为0.001851,最大值为0.2137,均小于1。结论内蒙古自治区部分地区鸡蛋样本中存在少量的土霉素和强力霉素残留,暴露风险较低,对人体健康危害处在可接受范围。