酶抑制法快速检测蔬菜中有机磷和氨基甲酸酯类农药残留的研究现状及展望

概述了酶抑制法快速检测蔬菜中有机磷和氨基甲酸酯类农药残留技术的研究现状、检测原理、应用情况和存在的问题。酶抑制法具有检测时间短、成本低、操作简便等特点,是目前我国控制农药残留的一种有效的初筛方法。     

Assessing the depletion of lincomycin in feathers from treated broiler chickens: a comparison with the concentration of its residues in edible tissues

ABSTRACT

Lincomycin is the first antimicrobial agent described for the lincosamide class and it is commonly used for the treatment of infectious enteric and respiratory diseases in poultry. Maximum residue limits (MRLs) in edible tissues have been established for this antimicrobial, however, no regulation has been proposed yet for by-products that are not intended for direct human consumption. Feathers are a by-product from poultry farming that might be used as an ingredient for diets fed to other farm animal species. The presence of antimicrobial residues in them is not monitored in spite of the fact that several studies have proved that they can persist in feathers. Currently though, no evidence has been presented regarding the behaviour of lincomycin in this matrix. Hence, this work intended to assess the depletion of lincomycin residues in feathers of birds treated with therapeutic doses and compare them with those detected in muscle and liver samples. Samples were collected for several days after ceasing treatment from a group of broiler chickens treated with a 25% lincomycin formulation. Methanol and Florisil® columns were used to extract and retain the analyte, and samples were analysed using a triple quadrupole mass spectrometer (API 5500, AB SCIEX?). On day 1 after ceasing treatment, average concentrations of lincomycin detected in feather samples reached up to 8582 μg kg^?1 and by day 16, these had only declined by 63%, to an average of 3138 μg kg^?1. Lincomycin residues were detected in feathers at every sampling point, even after they were not detectable in edible tissues. Depletion time was 98 days for feathers, considering the LOQ established for the methodology as cut-off value for the calculations. Data showed that lincomycin is highly persistent in feathers, which may result in this matrix becoming a re-entry route for its residues into the food chain.     

基于酶抑制法的农药残留快速检测仪器现状及评价

为了确保果蔬类农产品的食用安全, 对蔬菜瓜果进行农药残留的检测十分重要。本文通过对我国农药残留快速检测仪器的发展现状和评价方法的讨论, 分析了基于酶抑制法的农残速测仪器现存的主要问题, 并提出进行农残速测仪器评价工作的必要性。     

Improved microbial screening assay for the detection of quinolone residues in poultry and eggs

An improved microbiological screening assay is reported for the detection of quinolone residues in poultry muscle and eggs. The method was validated using fortified tissue samples and is the first microbial assay to effectively detect enrofloxacin, difloxacin, danofloxacin, as well as flumequine and oxolinic acid, at or below their EU maximum residue limits (MRL). The accuracy of the assay was shown by analysing incurred tissue samples containing residue levels around the MRL. Liquid chromatography-tandem mass spectrometry (LC-MS/MS) quantification of the quinolone concentration in these samples showed that the test plate can be used semi-quantitatively, allowing the definition of an “action level” as an inhibition zone above which a sample can be considered “suspect”. The presented assay is a useful improvement or addition to existing screening systems.     

在场拭子法检测猪组织中抗生素残留

目的建立在场拭子法(swab test on premises, STOP)并对深圳市不同来源的猪肉、猪肝和猪肾抗生素残留进行筛查。方法选用枯草芽孢杆菌CMCC-63501作为实验敏感菌株,通过测定猪肉组织的加标回收率、检出限和假阴性率建立STOP法,并对市售猪组织中抗生素残留量进行筛查。结果本研究建立了乳酸环丙沙星、盐酸多西环素、恩诺沙星、硫酸新霉素、头孢噻呋钠和硫酸庆大霉素共6种敏感抗生素的标准曲线。本研究建立的STOP法的加药回收率、检出限和假阴性率均符合方法学的要求。采用STOP法对不同来源猪肉、猪肝和猪肾中抗生素残留量的筛查,结果表明,猪肝和猪肾阳性超标率分别为24%和10%,这些样本均来源于郊区,其中农贸市场的风险要高于超市,而土猪和外三元的品种之间没有明显差异。结论猪组织抗生素残留风险高发的部位、区域和场所分别是内脏、郊区和农贸市场,与猪的品种没有明显的相关性。STOP法简单快捷易操作,可适用于动物性食品中抗生素残留的现场检测。     

免疫分析技术在金刚烷胺残留检测中的应用

文章总结并分析了应用于金刚烷胺残留检测中的酶联免疫、免疫层析、化学发光免疫分析技术等,并对其发展进行了展望。     

食品中莠去津残留检测方法的研究进展

莠去津是目前世界上使用范围最广、使用量最大的一种旱田除草剂,长期接触会损害人体健康,发展快速、简易、高灵敏检测食品中莠去津残留量的方法具有重要的现实意义。本文综述了近年来国内外食品中莠去津的主要检测技术及其研究进展,包括免疫分析法、色谱分析法和生物传感器法,对各种检测技术的检测原理、操作步骤及其各自的优缺点进行了比较分析。最后对食品中莠去津残留的检测技术在未来的发展方向作了展望。     

酶抑制法快速检测蔬菜中有机磷农药残留的最佳条件研究

采用酶抑制分光光度法快速检测蔬菜中有机磷农药残留,以抑制率为指标,研究了抑制时间、抑制温度、底物(碘化硫代丁酰胆碱)加入量和酶液加入量4个因素对检测条件的影响,通过正交试验和极差分析,得出4因素的主次关系为抑制时间>底物量>酶液量>温度,确定了蔬菜中有机磷农药残留的最佳检测条件为抑制时间15min、抑制温度35℃、底物加入量100μL、酶液加入量100μL。     

动物性食品中磺胺类药物残留检测研究进展

磺胺类药物因其具有抗菌谱广、价格低廉等特点,被广泛应用于兽药临床和畜牧业中。但磺胺类药物不合理使用导致其在动物产品中残留,严重危害人类健康。本文论述了动物性食品中磺胺类代谢物检测的样品前处理方法、仪器测定方法,综述了各检测方法的特性、适用范围及优缺点等。     

蜂产品中氯霉素残留检测方法的研究进展

本文综述了近年来蜂产品中氯霉素残留的主要检测方法及其研究进展, 包括微生物法、免疫分析法、色谱分析法和生物传感器法。其中, 免疫分析法着重介绍了酶联免疫法, 色谱分析法则主要介绍了高压液相色谱和色谱-质谱联用技术。最后, 对现有检测方法进行了比较分析。     

Evaluation and establishing the performance of different screening tests for tetracycline residues in animal tissues.

Four methods intended for screening muscle tissue for residues belonging to the tetracycline group were compared using artificially contaminated as well as incurred samples. Two agar diffusion methods were studied: one with Bacillus subtilis as a test strain, the second with Bacillus cereus. Two variants of each method were compared: thin plates for analysis of intact or minced meat, and thick plates for analysis of meat fluid. The thin plate variants could not be evaluated with artificially contaminated samples because it was impossible to prepare homogeneously spiked, undiluted meat. The thick plates were suited for doxycycline and chlortetracycline, but they did not detect oxytetracycline or tetracycline in spiked meat fluid. The results of these tests done on incurred meat were very good for doxycycline and satisfying or just failing for oxytetracycline, while the best detection capability was obtained when intact frozen meat was examined on thin plates seeded with B. cereus. Two commercially available screening tests were also evaluated. The Premi(R) test, an inhibitor test with Bacillus stearothermophilus as a test strain and an indicator for growth, was not suited for detection of tetracyclines up to the maximum residue limit. Tetrasensor(R), a receptor test specific for tetracyclines, proved a quick and simple test able to detect meat samples artificially contaminated with tetracycline, oxytetracycline, doxycycline or chlortetracycline, as well as meat incurred with oxytetracycline or doxycycline.     

农药残留快速检测用酶——胆碱酯酶的筛选

在常见易得的前提下,以猪血、鸡血、鸭血、链鱼和鸡肝为实验材料提取胆碱酯酶,通过比较不同来源、不同动物组织胆碱酯酶的活性,并进行了胆碱酯酶对常见农药的敏感性实验,结果表明:鸭血清BChE酶含量丰富、对常见的有机磷农药及氨基甲酸酯类农药较敏感、且来源广泛、廉价易得。可作为果蔬农药残留的快速检测用酶。     

动物源性食品中甲基睾酮残留检测方法研究进展

甲基睾酮是一种激素类药物,在畜牧业和水产养殖业中作为动物促生长剂和性别逆转剂而被使用。我国农业农村部235号公告规定了在所有动物组织中不得检出甲基睾酮,但是目前还存在违禁使用的情况,因此有必要对其残留量进行检测。本文主要概述了甲基睾酮的作用机制、危害和法规标准,系统综述了现有畜禽、水产品中甲基睾酮残留检测常用的样品前处理方法和分析方法。样品前处理方法的确定包括提取试剂的选择、净化方法的优化等,检测方法主要包括高效液相色谱法、液相色谱-串联质谱法、液相色谱/质谱联用法和免疫分析方法等。本文分析了不同检测方法的优缺点、适用范围以及选择依据,并对检测方法进行了展望,旨在为加强动物源性食品中甲基睾酮的残留监测提供参考。     

Development and validation of an immunochromatographic assay for the rapid detection of quinoxaline-2-carboxylic acid,the major metabolite of carbadox in the edible tissues of pigs

A new method was developed for the determination of quinoxaline-2-carboxylic acid, the marker residue of carbadox, in the edible tissues of food-producing animals using a colloidal gold probe-based immunochromatographic assay. The highly specific polyclonal antibody (PcAb), which was very sensitive to N-butylquinoxaline-2-carboxylic acid (BQCA) with an IC₅₀ value of 2.38?ng?ml^?1, was selected for the development of an immunochromatographic assay (ICA). Only 5?min were required to perform this assay; it had a visual detection limit of 25?ng?g^?1 for quinoxaline-2-carboxylic acid. The results of the analysis of quinoxaline-2-carboxylic acid in animal tissues using the immunochromatographic assay showed good agreement with those obtained by HPLC. In conclusion, the method was rapid and accurate for screening residues of carbadox in the edible tissues of food-producing animals.     

An improved microbial assay for the detection of chloramphenicol residues in shrimp tissues

An improved microbial assay was developed for the detection of chloramphenicol (CAP) residues in shrimp muscle using Photobacterium leiognathi (L-2 strain) isolated from squid, as test organism, using a pad plate technique. CAP spiked in shrimp muscle tissues at concentrations ranging from 1 to 100 μg/kg was extracted using ethyl acetate and ammonium hydroxide. The assay showed a maximum inhibition zone of 23.0 mm for 100 μg/kg and a minimum inhibition zone of 9.3 mm for 1 μg/kg. The method had a good recovery of 95.63% with a minimum detection limit of 1 μg/kg. It can be performed within 18 h following simple extraction. The method therefore proved to be advantageous over chromatographic procedures as it was inexpensive, quite sensitive and can be adopted for rapid screening of CAP in shrimp tissues.     

蔬菜中农药残留快速检测与定量检测结果符合性分析

目的验证蔬菜快速检测方法的有效性,提升其可信度。方法选取通过农药残留快速检测方法(酶抑制法)筛选出的结果呈阳性的样品,采用仪器分析法进行50项农药残留量的定量分析复核。从蔬菜品类检出符合率、不合格符合率,样品检出率、不合格符合率及各种农药的超标情况等方面进行数据分析。结果各类蔬菜中农药残留有检出样品占总体阳性样本的92%以上,检出符合率较高,表明快速筛查的阳性样品具有一定的风险;由于技术自身缺陷及部分农药缺少评价体系等原因,其不合格符合率为30%～50%左右,其中流通量较大的芸薹属类、叶菜类及茄果类蔬菜的不合格符合率分别为43.3%、33.6%、54.5%。结论快速检测技术作为蔬的农药残留初筛的手段是切实有效的,其应用对蔬菜的质量安全具有重要意义。     

动物源性食品中氟喹诺酮类抗生素残留检测方法的研究进展

氟喹诺酮类抗生素作为广谱高效抗菌药物应用在动物源性食品生产中。近年来,动物源性食品中抗生素残留也因其滥用而受到了广泛关注。为此,监管部门加大了对氟喹诺酮抗生素残留的监管力度。开展更加快速、高效、高灵敏度、高通量的检测动物源性食品中氟喹诺酮类残留的方法已成为对检测机构的新要求。本文就动物源性食品中氟喹诺酮类抗生素残留的检验方法的研究进展进行详细阐述,以期为动物源性食品质量监测、监管以及检测标准方法制定方面提供参考。     

Bioactive compounds and antioxidant capacities in different edible tissues of citrus fruit of four species

Different edible tissues of citrus fruit, namely juice sacs (JS), segment membrane (SM), and segment (Seg), of four species, were examined for contents of bioactive compounds and total antioxidant capacities (TAC) by ferric reducing antioxidant power (FRAP) assay. Two flavanones (naringin and hesperidin) were identified by HPLC; hesperidin accounted for 18.5–38.5% of the total phenolics in the species Citrus unshiu, Citrus reticulata, and Citrus sinensis, while naringin was only found in Citrus changshanensis and it accounted for 53.7% of the total phenolics in SM of this species. In SM of all selected species, the contents of phenolic compounds and TAC were significantly higher than those in JS and Seg. Highest total phenolics, total flavonoids, naringin, and TAC were found in SM of C. changshanensis, while the highest carotenoid content was found in JS of C. reticulata. The contribution of vitamin C to TAC ranged from 26.9% to 45.9% in JS and Seg of all selected species. In SM, however, a high contribution from hesperidin was observed in C. unshiu (54.0%), C. sinensis (46.7%) and C. reticulata (30.0%). The results indicated that SM of citrus fruit were high in contents of bioactive compounds and TAC; it is thus recommended to consume citrus fruit with all edible tissues rather than juice or JS alone.     

食用植物油中农药残留检测技术的研究进展

我国农产品中农药残留的中毒事件和进出口贸易中农药残留超标事件时有发生,已成为影响农业可持续发展的重要问题,因此农药残留检测技术也在迅速发展。文章综述了现阶段对植物油中农药残留检测技术的研究进展。主要从前处理和检测方法 2方面进行分析,根据前处理方法和检测方法的不同,分别介绍了各类前处理方法如液液萃取法(liquid-liquid extraction,LLE)、固相萃取法(solid phase extraction,SPE)、基质固相分散萃取法(matrix solid phase dispersion,MSPD)、分散固相萃取(disperse solid phase extraction,d SPE)法、凝胶渗透色谱法(gel permeation chromatography,GPC)等方法的原理和过程,以及各类检测方法如气相色谱法、气相色谱-质谱联用法(gas chromatography-mass spectrometry,GC-MS)、液相色谱法和液相色谱-串联质谱联用法(liquid chromatography-tandem mass spectrometry,LC-MS/MS)等的特点和应用范围。文章总结各类方法的优缺点,并提出了食用植物油中农药残留分析方法的发展趋势。