有机磷农药多残留检测化学发光标记物的合成及鉴定

目的以O,O-二乙基硫代磷酰氯和鲁米诺为原料,合成一种新型的化学发光标记物,用于后续的二乙氧基类有机磷农药多残留化学发光免疫法检测。方法取鲁米诺和O,O-二乙基硫代磷酰氯溶于二氯甲烷中,以三乙胺作为缚酸剂,冰浴下反应8 h后分出有机层,产物经柱层析纯化,即得到化学发光标记物。结果产物经紫外、红外鉴定,实验结果表明反应产物即为所需的化学发光标记物,产物在BPCL上进行发光特性测定,表现出较强的发光能力,最大发光强度达到9000 mV。结论本方法合成的化学发光标记物具有较强的发光能力,能用于后续的二乙氧基类有机磷农药多残留的化学发光免疫检测。     

化学发光法检测过氧化苯甲酰的研究

采用化学发光的方法检测过氧化苯甲酰,通过筛选体系找出合适的检测体系,并对所选检测体系的检测条件进行优化,初步确定化学发光法检测过氧苯甲酰的实验条件.实验结果表明,高锰酸钾浓度在1.8×10-5 mol/L(0.3 mol/L的硫酸介质),鲁米诺浓度在2.0×10-4 mol/L(pH7)时,过氧化苯甲酰在0～10×10-5h/mL内呈良好的线性关系,线性相关系数为0.9993,检出限为8×10-9g/mL.对浓度为3×10-5g/mL的过氧化苯甲酰平行测定20次,相对标准偏差(RSD)为1.32%.     

臭氧对有机磷农药残留降解效果及检测方法的研究

实验采用臭氧对敌敌畏、甲胺磷、久效磷、乙基对硫磷四种有机磷农药残留进行降解,并分别采用了酶抑制法和气相色谱法对其降解效果进行检测.结果表明,一定浓度的臭氧,作用不同时间,对上述四种有机磷农药残留均有不同程度的降解作用,作用10min即可达到较为理想的降解效果.其中,对甲胺磷降解作用最强为81.72%,敌敌畏57.86%、乙基对硫磷56.78%、久效磷47.53%.     

果蔬中残留有机磷农药降解菌的选育及鉴定

为减少果蔬中的农药残留量,利用96孔板从长期喷洒农药的耕地土壤中筛选出一株能高效降解有机磷农药的菌株,并对其进行形态学及生理生化鉴定,提取其基因组并与Gen Bank上已提交的26S r DNA进行BLAST比对,结果表明,其归属于红酵母菌属（Rhodotorula sp.）。由MEGA6.0软件构建的系统发育树结果表明,该菌株与Rhodotorula mucilaginosa 26S r DNA序列一致性可达99%,结果与生理生化实验相一致。因此,确定该菌株为胶红酵母菌（Rhodotorula mucilaginosa）,编号为RM-DY21。利用紫外分光光度法测定该菌株32 h内对毒死蜱（50 mg/L）降解率为70.04%。该菌株在以有机磷农药（毒死蜱、氧乐果和敌百虫）为唯一碳源的培养基中生长效果好,说明其对这三种农药均有降解效果,可以广泛降解有机磷农药。      

臭氧对有机磷农药残留降解效果及检测方法的研究

实验采用臭氧对敌敌畏、甲胺磷、久效磷、乙基对硫磷四种有机磷农药残留进行降解,并分别采用了酶抑制法和气相色谱法对其降解效果进行检测。结果表明,一定浓度的臭氧,作用不同时间,对上述四种有机磷农药残留均有不同程度的降解作用,作用10min即可达到较为理想的降解效果。其中,对甲胺磷降解作用最强为81.72%,敌敌畏57.86%、乙基对硫磷56.78%、久效磷47.53%。      

牛奶中有机氯农药及拟除虫菊酯农药多残留的HS-SPME-GC-MS分析方法研究

目的 建立牛奶中有机氯农药和拟除虫菊酯类农药的快速多残留测定方法.方法 以顶空固相微萃取作为前处理手段,采用气相色谱-质谱联用方法测定牛奶样品中31种农药组分（其中有机氯农药23种,拟除虫菊酯类农药8种）,并以13C6-六氯苯和13C10-灭蚁灵作为稳定的同位素内标物,采用内标法定量.结果 方法的最低检测限在0.002～0.2μg/L之间,回收率在85%～110%之间.相对标准差在3%～12%之间.结论 该方法快速、简单、准确、可靠、环保.适用于批量牛奶样品中农药残留的筛查.     

硬脂酰取代二羟乙基甘氨酸酯的合成及在造纸施胶中的应用研究

报道了一种新型的氨基酸类两性表面活性剂硬酯酰取代二羟乙基氨基酸酯的合成方法及其在造纸施胶中的应用效果研究.通过三步法反应合成目标产物,重点探讨酰氯酯化反应的各影响因素,确定合成最佳条件为:在无溶剂条件下,Bicine与硬酯酰氯的摩尔比为1:2,反应时间是8 h,反应温度为95℃.通过研究影响其应用效果的因素,证实其在pH值为5.5～7.5,助留剂CPAM用量w=0.5%,施胶剂用量w=1.0%,施胶效果理想.     

不同前处理对植物酯酶抑制法检测蔬菜中有机磷及氨基甲酸酯类农药残留的影响

利用酶抑制法可以快速检测蔬菜中的有机磷和氨基甲酸酯类农药残留,这两类农药能抑制酯酶的活性,并影响酯酶对底物的催化能力。根据这一原理,采用麦麸酯酶作为酶源对酶抑制法快速检测农残前处理方法中农残提取液、提取方法、提取时间及样品提取液的处理方式进行优化。结果表明:用5%丙酮-磷酸盐缓冲液作为提取液,然后超声提取5 min后,将样品提取液再用0.45μm有机滤膜过滤后蔬菜中农药残留提取量可达到最高;且样品加标回收率为83.61%~102.81%,变异系数为1.20%~7.23%。因此,该前处理方法可满足于麦麸酯酶抑制法快速检测农药残留的需要。     

食品中农药多残留检测新技术研究进展

食品安全是关系国计民生的大事, 发展农药残留检测新技术和开展食品中农药残留的风险评估有助于食品安全风险管理、风险交流和消费者健康。本文综述了多组分农药残留检测中最新的样品前处理方法、农药残留分析检测技术及其应用, 以期为农药残留分析检测技术的完善与发展提供参考与借鉴。     

Simultaneous determination of chloramphenicol,florfenicol and florfenicol amine in ham sausage with a hybrid chemiluminescent immunoassay

A novel chemiluminescent immunoassay utilising two types of primary antibodies (murine monoclonal antibody and rabbit polyclonal antibody) and two types of horseradish peroxidase–labelled secondary antibodies was established for simultaneously detecting multiple amphenicol residues in ham sausage. After combining the extract procedure of the target amphenicol into one simplified method, this hybrid chemiluminescent immunoassay could screen chloramphenicol (CAP), florfenicol (FF) and its metabolite florfenicol amine (FFA) at the same time by adding the corresponding secondary antibody. Ham sausage samples were analysed by using this hybrid immunoassay, with LODs of CAP being 0.01 μg kg^?1, of FF being 2.8 μg kg^?1 and of FFA being 3.0 μg kg^?1. The applicability of the proposed method has been validated by determining CAP, FF and FFA in ham sausage samples with satisfactory results. Good recoveries and high correlation with traditional enzyme-linked immunosorbent assay and LC-MS/MS results illustrated that the developed hybrid chemiluminescent immunoassay could screen high-throughput ultra-trace amphenicol residues effectively at one time.     

有机磷及氨基甲酸酯类农药残留检测方法研究进展

目前在中国蔬菜中农药残留最为严重的是有机磷类和氨基甲酸酯类农药。该文主要综述了有机磷及氨基甲酸酯类农药检测技术中广泛使用的光谱法及色谱法。     

分子标记技术及其在益生菌分类中的应用

益生菌的准确分类鉴定是益生菌应用于功能食品、药品开发的前提。由于益生菌菌群结构的多样性和复杂性,传统方法如形态结构、培养特征试验和生理生化试验等对其组成的研究准确性低且耗时长。随着分子生物学技术的发展,现代分子标记技术的应用为益生菌分类研究提供了一个新的方向。该文对常用的分子标记技术进行了概括包括分子杂交标记、PCR分子扩增标记和新型分子标记。以益生菌菌群分类鉴定为例,分析分子标记技术的基本原理、特点和现状,为其进一步开发提供基础。     

Evolution and perspectives of cultivar identification and traceability from tree to oil and table olives by means of DNA markers

In recent years, an increasing number of typicality marks has been awarded to high‐quality olive oils produced from local cultivars. In this case, quality control requires effective varietal checks of the starting materials. Moreover, accurate cultivar identification is essential in vegetative‐propagated plants distributed by nurseries and is a pre‐requisite to register new cultivars. Food genomics provides many tools for cultivar identification and traceability from tree to oil and table olives. The results of the application of different classes of DNA markers to olive with the purpose of checking cultivar identity and variability of plant material are extensively discussed in this review, with special regard to repeatability issues and polymorphism degree. The characterization of olive germplasm from all countries of the Mediterranean basin and from less studied geographical areas is described and innovative high‐throughput molecular tools to manage reference collections are reviewed. Then the transferability of DNA markers to processed products – virgin olive oils and table olives – is overviewed to point out strengths and weaknesses, with special regard to (i) the influence of processing steps and storage time on the quantity and quality of residual DNA, (ii) recent advances to overcome the bottleneck of DNA extraction from processed products, (iii) factors affecting whole comparability of DNA profiles between fresh plant materials and end‐products, (iv) drawbacks in the analysis of multi‐cultivar versus single‐cultivar end‐products and (v) the potential of quantitative polymerase chain reaction (PCR)‐based techniques. © 2016 Society of Chemical Industry     

利用拉曼光谱技术识别溴氰菊酯和 啶虫脒农药的研究

目的 初步建立溴氰菊酯农药和啶虫脒农药的拉曼光谱研究方法。方法 利用激光拉曼光谱技术, 将农药溶液装满铝盒, 采集农药溶液的拉曼光谱曲线, 运用自主编写的程序对光谱曲线进行预处理, 以去除光谱噪音并扣除荧光背景, 进而探讨溴氰菊酯农药和啶虫脒农药的快速无损检测方法。结果 溴氰菊酯农药和啶虫脒农药的拉曼特征频率较为丰富, 选取574 cm?1、736 cm?1处的拉曼信号可识别溴氰菊酯农药, 检测限为2500 mg/kg。选取752 cm?1、840 cm?1处的拉曼信号可识别啶虫脒农药, 当溶剂的丙酮-水比例为1:5时, 最适合作为检测溶剂配置啶虫脒农药溶液, 为下一步确定啶虫脒检测限奠定基础。结论 本研究对实现拉曼光谱技术检测果蔬表面溴氰菊酯农药和啶虫脒农药具有重要意义。     

Development of a chemiluminescent enzyme‐linked immunosorbent assay for five sulfonamide residues in chicken muscle and pig muscle

BACKGROUND: An enzyme‐linked immunosorbent assay (ELISA) based on polyclonal antibodies with enhanced chemiluminescent (ECL) detection of sulfonamides in food samples has been optimised and characterised. The specificity of the assay was assessed by determining cross‐reactivities with a set of 16 sulfonamides. The aim of this study was to develop a method for determining sulfonamides with high sensitivity. RESULTS: The sensitivity of the developed ECL‐ELISA was higher than that of colorimetric ELISA. The sensitivities of five of the sulfonamides (sulfisozole, sulfathiazole, sulfameter, sulfamethoxypyridazine and sulfapyridine) ranged from 0.73 to 2.92 µg L^?1, with limits of detection of 0.10–0.43 µg L^?1. The coefficients of variation of intra‐assay and inter‐assay studies carried out over 5 days were mostly less than 10%. Recovery studies of chicken muscle and pig muscle were performed with simple and rapid extraction. Good recoveries (62.1–110.3%) were achieved and the results correlated well with those obtained using high‐performance liquid chromatography analysis. CONCLUSION: This study has provided an effective analytical technique for the rapid and reliable determination of residues of sulfisozole, sulfathiazole, sulfameter, sulfamethoxypyridazine and sulfapyridine in food samples with high sensitivity. To the authors' knowledge, this is the first report on chemiluminescent ELISA for sulfonamide analysis. Copyright © 2008 Society of Chemical Industry     

Simultaneous determination of aging markers in sugar cane spirits

In this work a method for simultaneous determination of 10 representative compounds in sugar cane spirits is reported. The low molecular weight phenolic compounds: gallic acid; vanillic acid; syringic acid; vanilin; syringaldehyde; coniferaldehyde; sinapaldehyde and coumarin; and the furanic aldehydes: 5-hydroxymethyl-furfural and furfural were simultaneously quantified by high performance liquid chromatography with UV detection. These compounds, together with acids, aldehydes and tannins are responsible for the organoleptic properties of aged beverages and can assest product quality, as well as be used as aging indicators. Determination of this group of compounds is important, as they are characteristic of types and styles of aged beverages.     

Simultaneous determination of organophosphorus pesticides in cruciferous vegetables by dual-column GC with pulsed FPD and FTD

We evaluated simultaneous analytical methods for organophosphorus pesticides in cruciferous vegetables by gas chromatography (GC). Firstly, 36 pesticides were selected on the basis of monitoring data (April 1996-March 2003) in Aichi Prefecture. A sample was extracted with acetonitrile and the acetonitrile layer was separated by salting-out. The extract was cleaned up with gel permeation chromatography (GPC), and then with a tandem silica-gel/PSA mini-column. The test solution was subjected to dual-column GC equipped with a pulsed FPD (P mode, Rtx-OPPesticides column) and a FTD (Rtx-OPPesticides 2 column). Organophosphorus pesticides in such sulfur-rich matrices as cabbage and radish were determined without any serious interfering peaks on the pulsed FPD chromatograms after diluting the extracts 10- to 20-fold (0.25-0.5 mg/L of sample). The method was applied to cruciferous vegetables to demonstrate its usefulness in routine analysis.