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.

Determination of Residues and Safety Analysis of Metal Impurities in Platinum-based Antitumor Drugs

The residual metal impurities in cisplatin, carboplatin and oxaliplatin were determined by ICP-AES. The samples were ignited and dissolved with HCl:HNO 3 (3:1). The method is simple and accurate. By the determination of the metal residues in the samples, the calculated actual daily exposure and concentration of the metal Pd, Ir, Rh, Ru, Mo, Ni, Cr, V, Cu, Mn, Fe and Zn that were less than the permitted daily exposures (PDE) and the limited concentration permitted in the EMEA guideline on the specification limits for residues of metal catalysts or metal reagents [1] . The metal residues can de adequately removed from the active pharmaceutical ingredients and the corresponding drugs. The trace metal residues will not affect human health and lead to the safety hazard by the intravenous injection.

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.

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.

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.

Analysis of spironolactone residues in industrial wastewater and in drug formulations by cathodic stripping voltammetry

The redox behavior of spironolactone（SP） drug in Britton-Robinson（BR） buffer of pH 2-11 was investigated by differential pulse cathodic stripping voltammetry（DPCSV） and cyclic voltammetry（CV） at hanging mercury dropping electrode（HMDE）.At pH 9-10.5,the DPCSV of SP drug showed two cathodic peaks at1.15 and1.38 V at the HMDE vs.Ag/AgCl reference electrode.In the CV,at pH 9-10,the dependence of the cathodic peak current,Ip,c and peak potential,Ep,c of the second peak（Ep,c2） on the scan rate（n） and on the depolizer（SP） concentrations was typical of an electrode coupled（EC） chemical reaction type mechanism.The plot of Ip,cat 1.380 V of the DPCSV vs.SP concentration at pH 9 was linear over the concentration range of 1.2×1010-9.6×107 M.The lower limit of detection（LLOD） and limit of quantification（LOQ） of the drug were 1.1×1011 and 4.14×1011 M,respectively.The method was successfully applied for the analysis of SP residues in industrial wastewater,in pure form（98.273.1%） and in drug formulations e.g.Aldactones tablet（98.3572.9%）.The method was validated by comparison with HPLC and the official data methods.

Selection of Test Samples for Monitoring Veterinary Drug Residue in Bred Animals

[Objective] This study aimed to compare the residue situation of cimaterol,a kind of forbidden veterinary drug in hair, urine and flesh of pig, so as to provide theoretical basis for monitoring veterinary drug residue in bred animals. [Method]Total three different concentrations of cimaterol were administered to pigs, and the residue amounts of cimaterol in pig hair, urine and flesh were monitored at different raising stage. [Result] During the administration period, the residue amount of cimaterol was highest in urine, so urine is the suitable sample for rapid detection of cimaterol in manufacturing enterprises. Cimaterol could be accumulated in pig hair,where cimaterol was metabolized slowly. Thus, pig hair can be used as the test sample for tracing illegal use of veterinary drugs and for vivo detection. Flesh can be used as test sample for direct judgment whether cimaterol residue exceeds the relevant standard. [Conclusion] This study will provide certain theoretical basis for drug monitor in animal husbandry.

Chromatoprobe as a sample-sparing technique for residual solvent analysis of drug discovery candidates by gas chromatography

In drug discovery research, residual solvent measurement is an integral part of purity analysis for synthesis of a drug candidate before it is used for toxicity testing. This is usually carried out using gas chromatography(GC)with direct injection sample introduction. This method requires testing compounds to be soluble at high concentrations( > 50 mg/mL, usually in DMSO) to achieve acceptable sensitivity, a hurdle which is not always achievable for some samples such as cyclic peptides and oligonucleotides. To overcome the limitation associated with the direct injection approach, a new method using the Chromatoprobe thermal extraction device was developed for quantifying residual solvents of drug discovery compounds. This method not only consumes significantly less material(less than 1 mg), but also shows higher sensitivity than the direct injection approach.In addition, because no diluent is required with the Chromatoprobe thermal extraction, all residual solvents can be detected and measured without further method optimization. In our study, we compared data from GC residual solvent analysis using the Chromatoprobe solid sample introduction to those of the direct injection method for seven in-house samples. Our results showed a good agreement between the data from these two sample introduction methods. Thus, the Chromatoprobe sample introduction method provided a samplesparing alternative to the direct injection method for the measurement of residual solvents in drug discovery.This method can be particularly useful for residual solvent analysis in samples that are available only in limited amounts, poorly soluble, and/or unstable in the diluents used for the direct injection method.

Antibiotic residues in milk and milk products:A momentous challenge for the pharmaceutical industry and medicine

Dairy products are nutritious food items that contain various essential nutrients,however,it has been proven that residual antibiotics have contaminated such products.These residues can cause several side effects on human health.They increase antimicrobial resistance against several threatening microorganisms,as well as significant growth in allergenic reactions.Various methods,including heat treatments,have been applied to alleviate and reduce the effect of antibiotic residue level in milk and milk products.Changes in drug levels were not sig-nificantly remarkable,obliging researchers to find new approaches to prevent or reduce their risk and limit their complications on human health.

A COVID-19 Detection Model Based on Convolutional Neural Network and Residual Learning

Amodel that can obtain rapid and accurate detection of coronavirus disease 2019(COVID-19)plays a significant role in treating and preventing the spread of disease transmission.However,designing such amodel that can balance the detection accuracy andweight parameters ofmemorywell to deploy a mobile device is challenging.Taking this point into account,this paper fuses the convolutional neural network and residual learning operations to build a multi-class classification model,which improves COVID-19 pneumonia detection performance and keeps a trade-off between the weight parameters and accuracy.The convolutional neural network can extract the COVID-19 feature information by repeated convolutional operations.The residual learning operations alleviate the gradient problems caused by stacking convolutional layers and enhance the ability of feature extraction.The ability further enables the proposed model to acquire effective feature information at a lowcost,which canmake ourmodel keep smallweight parameters.Extensive validation and comparison with other models of COVID-19 pneumonia detection on the well-known COVIDx dataset show that(1)the sensitivity of COVID-19 pneumonia detection is improved from 88.2%(non-COVID-19)and 77.5%(COVID-19)to 95.3%(non-COVID-19)and 96.5%(COVID-19),respectively.The positive predictive value is also respectively increased from72.8%(non-COVID-19)and 89.0%(COVID-19)to 88.8%(non-COVID-19)and 95.1%(COVID-19).(2)Compared with the weight parameters of the COVIDNet-small network,the value of the proposed model is 13 M,which is slightly higher than that(11.37 M)of the COVIDNet-small network.But,the corresponding accuracy is improved from 85.2%to 93.0%.The above results illustrate the proposed model can gain an efficient balance between accuracy and weight parameters.

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。

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。

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。

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。

基于不同识别元件的β-内酰胺类药物快速检测方法研究进展

β-内酰胺类药物被广泛用于动物细菌性疾病的治疗,在世界抗生素市场中占据了超过一半的份额。然而,此类药物给食品动物大量使用会造成在动物源性食品中的残留,从而对消费者健康构成潜在威胁。因此,必须要对此类药物在动物源性食品中的残留进行检测。在β-内酰胺类药物的快速检测方法中,核心试剂是使用识别元件,它直接影响检测方法的选择性。受体、抗体、适配体、分子印迹聚合物等识别元件均具有特异性识别能力,已被用于不同兽药的残留检测。本文着重论述了近年来基于上述识别元件的方法在β-内酰胺类药物残留检测方面的应用,旨在为相关研究人员提供一些帮助。

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。

福州城区内河主要野生鱼类体内抗菌药物残留调查与分析

目的:为更好评价福州内河治理后的生态环境,在福州城区内河首次开展主要野生鱼体内6类抗菌药物残留调查。方法:以光明港、晋安河、白马河和凤坂河等4条福州主要内河水系为调查对象,共布设11个调查站位;并分别于2021年12月和2022年6月共采集27份样品,参照GB/T 22955-2008、GB/T 20762-2006等标准方法进行检测。调查结论:福州城区内河生态环境未受大部分常用抗菌药物污染,总体情况良好。

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。

“三全育人”视角下高职《药物残留检测技术》课程教学探索与实践

课程思政是新时代中国高等教育的理论创新与实践创新,是构建全员、全程、全方位育人即“三全育人”格局的有力抓手。依托高职院校药品质量与安全专业群建设,对《药物残留检测技术》课程思政育人的必要性、存在问题和教学改革进行研究,探索通过设立体系化的课程思证目标、优化课程思政教学设计、提升专业课教师课程思政教学能力、建立科学实效性的课程思政教学质量评价体系充分发挥课堂教学的育人功能,促进高职院校专业教育与政治思想教育同向同行。