高效液相色谱法同时测定水产品中13种磺胺类药物残留的研究

建立了一种同时测定水产品(鳗鱼、鮰鱼、龙虾)中13种磺胺类药物残留的高效液相色谱法。样品经乙腈提取,正己烷液-液分配,阳离子固相萃取小柱净化后,采用高效液相色谱分离,紫外检测器检测,外标法定量。13种磺胺类药物在0.1～5.0μg/ml范围内线性关系良好,相关系数R2为0.9997～0.9999,加标回收率为62%～97%,相对标准偏差为2.01%～10.46%。定量测定低限磺胺二甲嘧啶、磺胺甲氧嘧啶、磺胺-6-甲氧嘧啶、磺胺氯哒嗪、磺胺甲基异恶唑、磺胺二甲异恶唑、磺胺间二甲氧嘧啶、磺胺喹恶啉为0.02mg/kg,磺胺嘧啶、磺胺吡啶、磺胺噻唑、磺胺甲基嘧啶、磺胺甲噻二唑为0.05mg/kg。     

鸡蛋中7种磺胺药物的多残留检测方法研究

本试验研究建立了高效液相色谱法测定鸡蛋中7种磺胺药物（磺胺嘧啶、磺胺二甲基嘧啶、磺胺甲氧哒嗪、磺胺间甲氧嘧啶、磺胺甲恶唑、磺胺间二甲氧嘧啶和磺胺喹恶啉）残留的提取、净化和高效液相色谱分析条件，鸡蛋经二氯甲烷提取、固相萃取、净化处理后上机检测，7种磺胺药物标准曲线的相关系数（R^2）为0．9995～0．9999，在0．05～0．2mg／kg浓度范围内，回收率为73．2％-102．6％，变异系数为1．8％～8．7％。检测限为0．01～0．02mg／kg，定量限低于0．05mg／kg。     

高效液相色谱-荧光检测法测定水产品中4种磺胺类药物残留量

建立高效液相色谱-荧光检测法测定水产品中4种磺胺类药物残留量的方法。均质后的样品用乙酸乙酯提取,稀盐酸反萃取,正己烷脱脂,荧光胺衍生,反相色谱柱分离,荧光检测器检测,磺胺5-甲氧嘧啶为内标物,内标法定量。4种磺胺类药物磺胺嘧啶、磺胺甲基嘧啶、磺胺二甲基嘧啶和磺胺甲基异噁唑的线性范围为0.01～0.2mg/kg,线性相关系数均大于0.9934;在0.01～0.2mg/kg 范围内四个添加水平范围内的平均回收率为83.0%～91.3%,相对标准偏差为3.89%～8.80%,方法检出限为0.01mg/kg。     

液相色谱-荧光检测法同时测定肠衣中八种磺胺类兽药残留

建立了一种专属性强的高效液相色谱-同时测定肠衣中八种磺胺类药物残留(磺胺嘧啶、磺胺间甲氧嘧啶、磺胺甲基嘧啶、磺胺对甲氧嘧啶、磺胺喹恶啉、磺胺甲基异恶唑、磺胺甲氧嗪和磺胺二甲嘧啶)的检测方法。采用1%乙酸/乙腈对肠衣中的磺胺类药物残留进行提取,用正己烷净化,净化后的样品,经荧光胺衍生,供液相色谱仪测定。实验结果表明,八种磺胺药物在2.00～5.00×102ng/ml浓度范围内,具有良好的线性关系,线性相关系数在0.9982～0.9997,添加浓度为5～50ng/ml时,回收率在63.7%～87.8%之间,该方法的最低检测限为5ng/ml,完全可以达到日常检测要求。     

基质固相分散-高效液相色谱法测定蜂蜜中10种磺胺类药物

目的 建立基质固相分散一高效液相色谱法测定蜂蜜中10种磺胺类药物残留量的方法,包括磺胺、磺胺嘧啶、磺胺吡啶、磺胺甲基嘧啶、磺胺二甲基嘧啶、磺胺甲氧嘧啶、磺胺间甲氧嘧啶、磺胺氯哒嗪、磺胺甲噁唑和磺胺二甲异噁唑.方法 蜂蜜样品与C,:固相吸附荆于玻璃研钵中研磨均匀,得半干状混合物,装入空的固相萃取管中,盖上一层滤纸,以1+3二氯甲烷-乙酸乙酯(V/V)为洗脱剂洗脱,洗脱液经氮气吹干,用流动相溶解残渣,经0.45 μtm滤膜过滤,Agilent TC-C_18(4.6 mm×250 mm,5μm)色谱柱分离,高效液相色谱法测定.结果 10种磺胺类药物的线性范围为0.10～10.00 mg/L,相关系数r > 0.999,样品加标回收率60.0%～109.3%,相对标准偏差小于10%,方法检出限0.016-0.025 mg/L,样品中磺胺类检出限为0.050～0.079 mg/kg.     

RP-HPLC快速分析牛奶中六种磺胺类抗生素残留

研究了牛奶中磺胺嘧啶、磺胺甲基嘧啶、磺胺二甲基嘧啶、磺胺甲噁唑、磺胺间甲氧嘧啶、磺胺二甲氧嘧啶六种磺胺类抗生素的多残留反相高效液相色谱(RP-HPLC)分析方法.样品经超声波提取两次,提取液浓缩至干.残渣用流动相甲醇-0.08%乙酸(60:40,V/V)溶解,净化后以反相C18柱,甲醇-0.08%乙酸等度洗脱,紫外检测器检测、外标法定量.结果表明,这六种抗生素在0.01～1.0mg·L-1浓度范围内呈线性关系,磺胺嘧啶、磺胺甲基嘧啶、磺胺二甲基嘧啶的栓出限为0.010mg·L-1、磺胺甲噁唑、磺胺间甲氧嘧啶、磺胺间二甲氧嘧啶的检出限为0.015mg·L-1.分析的添加回收率达到80%以上,变异系数＜9.0%,整体分析时间小于3h.方法具有处理简单、检测快速、准确的特点.     

牛奶中多种磺胺类抗生素残留的HPLC快速分析

研究了牛奶中磺胺嘧啶、磺胺甲基嘧啶、磺胺二甲基嘧啶、磺胺甲噁唑、磺胺间甲氧嘧啶、磺胺二甲氧嘧啶六种磺胺类抗生素的多残留高效液相色谱(HPLC)分析方法。样品经氯仿-丙酮(2:1,V/V)提取两次,提取液浓缩至干。残渣用流动相甲醇-0.08%乙酸(60:40,V/V)溶解,净化后以反相C18柱,甲醇-0.08%乙酸等度洗脱,紫外检测器检测、外标法定量。结果表明,这六种抗生素在0.01～1.0mg/L浓度范围内呈线性关系,磺胺嘧啶、磺胺甲基嘧啶、磺胺二甲基嘧啶检的检出限为0.010mg/L、磺胺甲噁唑、磺胺间甲氧嘧啶、磺胺间二甲氧嘧啶检出限分别为0.015mg/L。分析的添加回收率为69.4%～123.5%,变异系数为<8%,整体分析时间小于3h。方法具有处理简单、检测快速、准确的特点。     

海参中十种磺胺类药物残留量的高效液相色谱检测

旨在利用高效液相色谱法检测海参中磺胺类药物(SAS)的残留量。样品前处理经过二氯甲烷提取和正己烷净化两步,净化后的样品以高效液相色谱仪测定。选用十种磺胺类药物作为标准品,色谱柱采用ZORBAX SB-C18色谱柱,乙腈∶水∶冰醋酸=18∶81∶1梯度洗脱,流速1.0mL/min,柱温45℃,紫外285nm处检测,线性范围0.064～0.832μg/mL(r=0.9801～0.9967),十种SAS都能得以有效分离,海参样品中检出磺胺嘧啶、磺胺噻唑、磺胺甲氧哒嗪三种磺胺类药物,此方法准确可靠。     

高效液相色谱-在线柱后衍生荧光检测法同时测定水产品中14种磺胺类药物残留

建立水产品中14种磺胺类药物的高效液相色谱-柱后衍生荧光检测法。均质后的水产品试样用乙酸乙酯提取、盐酸溶液反萃取、正己烷脱脂、反相色谱柱分离、在线柱后衍生、荧光检测器检测、内标法定量。14种磺胺类药物(磺胺、磺胺嘧啶、磺胺噻唑、磺胺甲基嘧啶、磺胺5-甲氧嘧啶、磺胺二甲基嘧啶、磺胺甲氧哒嗪、磺胺氯哒嗪、磺胺6-甲氧嘧啶、磺胺甲基异噁唑、磺胺多辛、磺胺异噁唑、磺胺二甲氧哒嗪、磺胺喹噁啉)的线性范围为2.5～800μg/L,线性相关系数均大于0.9934;在2.5～200μg/kg三个添加水平范围内的平均回收率为88.9%～98.6%,相对标准偏差均小于6.96%。14种磺胺类药物的定量检出限为2.5～20μg/kg。方法重现性好、灵敏度高,杂质干扰少,广泛适用于水产品中磺胺类药物残留的检测。     

高效液相色谱-串联质谱法同时测定漱口水中的11种磺胺类药物

目的 建立一种高效液相色谱-串联质谱法(high performance liquid chromatography tandem mass spectrometry, HPLC-MS/MS)同时测定漱口水中11种磺胺类药物(磺胺嘧啶、磺胺噻唑、磺胺吡啶、磺胺甲基嘧啶、磺胺甲噻二唑、磺胺氯哒嗪、磺胺甲基异噁唑、磺胺二甲异噁唑、磺胺喹噁啉、磺胺硝苯、磺胺苯吡唑)残留的方法。方法 样品经超声提取后, 以Agilent Eclipse XDB-C18(10 cm×4.6 mm, 3.5 μm)色谱柱分离后在高效液相色谱-串联质谱法多反应监测模式下进行测定, 外标法定量。结果 11种磺胺类药物的检出限为15 μg/kg, 在3个添加水平范围内的平均回收率为80.3%~105.4%, 相对标准偏差均小于8.5%。结论 该方法简便、准确, 快速, 适用于漱口水中磺胺类药物的测定。     

微波消化法测定鳗鱼中痕量铅的最佳条件研究

采用微波消化-原子吸收光谱法测定鳗鱼中痕量铅。研究铅含量随着微波消化的压力、时间、混合酸比例及称样量等因素的变化而变化的规律,并通过单因素及正交试验确定了微波消解鳗鱼的最佳条件,即微波压力为2MPa、作用时间为10min、混合酸的比例为6∶2、称样量为0.2g,283.30nm波长处铅的检出限为0.008mg/kg(3s),线性范围为0～80μg/L,样品分析结果的相对标准偏差2.6%(n=7),加标回收率在95%～105%,该法简便、快速、灵敏、准确、线性范围宽。     

鳗鱼油胶囊改善记忆作用的研究

为研究昂泰鳗鱼油改善记忆的作用,通过跳台试验、避暗试验、水迷宫试验３种方法,观察鳗鱼油对小鼠行为记忆的影响,经口给予小鼠０、１５０、３００、９００ｍｇ／ｋｇＢＷ剂量的受试物３０ｄ,结果表明：对小鼠的被动回避反应及空间辨别能力的记忆获得和再现有改善作用;采用韦氏记忆量表法进行双盲法人体试食实验,结果表明：每天早、晚各服用鳗鱼油胶囊１．２ｇ,连续３０ｄ,对改善人体学习记忆有一定作用。     

HPLC法测定鳗鱼中三种喹诺酮药物残留

目的建立一种高效液相色谱方法测定鳗鱼中环丙沙星、恩诺沙星和恶喹酸3种喹诺酮类药物残留量,方法试样用含1％乙酸的乙腈提取,用正己烷脱脂、浓缩,缓冲盐＋乙腈（80＋20,体积分数）溶解,超高速离心净化,用荧光检测器测定,外标法峰面积定量。结果试样在10、0～60．0μg／kg范围内校正曲线呈良好的线性关系,3种物质的相关系数都在0．999以上。加标回收率：恶喹酸为87．4％～105．1％,环丙沙星为70．0％～85．7％,恩诺沙星为76.0％～92．8％,相对标准偏差均小于10％;检出限：恶喹酸为1.4μg／kg,环丙沙星为2．7μg／kg,恩诺沙星为1．5μg／kg。结论该方法操作简单、快捷．结果准确、可靠。     

超高效液相色谱-串联质谱法同时测定鳗鱼中32种兽药残留

目的 建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)同时测定鳗鱼中13种磺胺类、15种喹诺酮类和4种四环素类兽药残留的分析方法。方法 鳗鱼试样采用乙二胺四乙酸二钠(ethylenediaminetetraacetic acid disodium salt, Na2EDTA)-Mcllvaine提取液进行提取, HLB固相萃取柱净化, Waters ACQUITY UPLC BEH C18色谱柱分离, 以0.1%甲酸乙腈和0.1%甲酸水溶液作为流动相进行梯度洗脱; 电喷雾正离子模式下, 以多反应监测(multiple reaction monitoring, MRM)方式采集数据进行定性与定量分析, 外标法定量。结果 磺胺类、喹诺酮类及四环素类药物分别在2~50、2~50、5~100 μg/kg浓度范围内线性相关性良好, 相关系数均大于0.99; 不同加标水平的平均回收率为82.6%~110.2%, 相对标准偏差(relative standard deviations, RSDs)为3.2%~13.9%, 检出限(limits of detection, LODs)和定量限(limits of quantification, LOQs)分别为0.3~2.0 μg/kg和1.0~5.0 μg/kg。结论 本方法快速简便、灵敏可靠, 适合大批量鳗鱼中同时快速对磺胺类、喹诺酮类及四环素类兽药残留进行定性和定量检测。     

Brominated,chlorinated and mixed brominated/chlorinated persistent organic pollutants in European eels (Anquilla anquilla) from Latvian lakes

Fifty-eight European eel (Anquilla anquilla) specimens collected from five Latvian lakes were investigated for six groups of persistent organic pollutants (POPs), including polychlorinated, polybrominated and mixed bromo-chloro dibenzo-p-dioxins and dibenzofurans (PCDD/DFs, PBDD/DFs and PXDD/DFs), polychlorinated and mixed bromo-chloro biphenyls (PCBs and PXBs) and polybrominated diphenyl ethers (PBDEs). PCDD/DFs and PCBs were found to occur in the range 0.85–15.8 pg Total-WHO₂₀₀₅-TEQ g^?1 f.w., and concentrations in most of the samples were below the maximum levels specified in European Commission Regulation (EU) No. 1259/2011. The summed concentrations of 27 PBDEs (∑_PBDE) and 16 non-dioxin-like PCBs (∑_NDL-PCB) were in the ranges of 0.28–26.7 and 6.37–320 ng g^?1 f.w., respectively. PBDD/DFs, PXDD/DFs and PXBs show average upper-bound concentrations of 0.05, 0.06 and 0.01 pg TEQ f.w. and collectively contributed 3.4% to the sum TEQ of dioxin-like compounds. The highest contaminant concentrations were measured in samples from lakes near the Baltic Sea and the industrialised area near Riga (Liepajas and Kisezers lakes). A correlation of POP concentration with the length of collected specimens was observed.     

Simultaneous Determination of Malachite Green,Diethylstilbestrol, Medroxyprogesterone,and 3-Amino-2-Oxazolidone in Synbranchoid Eels by a Protein Microarray Method

Food Analytical Methods - Protein chips have emerged as a useful approach for a wide variety of applications, including the identification of small molecule targets. In this study, a protein...     

Textural Properties of Cold-set Gels Induced from Heat-denatured Whey Protein Isolates

A 9% whey protein (WP) isolate solution at pH 7.0 was heat-denatured at 80°C for 30 min. Size-exclusion HPLC showed that native WP formed soluble aggregates after heat-treatment. Additions of CaCl2 (10–40 mM), NaCl (50–400 mM) or glucono-delta-lactone (GDL, 0.4–2.0%, w/v) or hydrolysis by a protease from Bacillus licheniformis caused gelation of the denatured solution at 45°C. Textural parameters, hardness, adhesiveness, and cohesiveness of the gels so formed changed markedly with concentration of added salts or pH by added GDL. Maximum gel hardness occurred at 200 mM NaCl or pH 4.7. Increasing CaCl2 concentration continuously increased gel hardness. Generally, GDL-induced gels were harder than salt-induced gels, and much harder than the protease-induced gel.     

Occurrence of bisphenol-F-diglycidyl ether (BFDGE) in fish canned in oil

The levels of bisphenol-F-diglycidyl ether (BFDGE) were quantified as part of a European survey on the migration of residues of epoxy resins into oil from canned fish. The contents of BFDGE in cans, lids and fish collected from all 15 Member States of the European Union and Switzerland were analysed in 382 samples. Cans and lids were separately extracted with acetonitrile. The extraction from fish was carried out with hexane followed by re-extraction with acetonitrile. The analysis was performed by reverse phase HPL C with fluorescence detection. BFDGE could be detected in 12% of the fish, 24% of the cans and 18% of the lids. Only 3% of the fish contained BFDGE in concentrations considerably above 1mg/kg. In addition to the presented data, a comparison was made with the levels of BADGE (bisphenol-A-diglycidyl ether)analysed in the same products in the context of a previous study.     

Contribution of European research to risk analysis

The European Commission's, Quality of Life Research Programme, Key Action 1—Health, Food & Nutrition is mission-oriented and aims, amongst other things, at providing a healthy, safe and high-quality food supply leading to reinforced consumer confidence in the safety of European food. Its objectives also include the enhancing of the competitiveness of the European food supply. Key Action 1 is currently supporting a number of different types of European collaborative projects in the area of risk analysis. The objectives of these projects range from the development and validation of prevention strategies including the reduction of consumers risks; development and validation of new modelling approaches; harmonization of risk assessment principles, methodologies, and terminology; standardization of methods and systems used for the safety evaluation of transgenic food; providing of tools for the evaluation of human viral contamination of shellfish and quality control; new methodologies for assessing the potential of unintended effects of genetically modified (genetically modified) foods; development of a risk assessment model for Cryptosporidium parvum related to the food and water industries; to the development of a communication platform for genetically modified organism, producers, retailers, regulatory authorities and consumer groups to improve safety assessment procedures, risk management strategies and risk communication; development and validation of new methods for safety testing of transgenic food; evaluation of the safety and efficacy of iron supplementation in pregnant women; evaluation of the potential cancer-preventing activity of pro- and pre-biotic ('synbiotic') combinations in human volunteers. An overview of these projects is presented here.     

低温带皮菜籽粕微粉的不同粒级部分的功能特性

为研究低温带皮菜籽粕微粉的不同粒级部分的功能特性,以经低温脱脂的带皮菜籽粕为原料,经微粉碎后筛分成212~425μm、150~212μm和106~150μm的3个不同粒级的微粉样品,检测这些样品的吸水性、吸油性、乳化性和乳化稳定性、蛋白质体外消化率。结果表明:1 3个不同粒级的微粉样品之间的粗纤维含量存在显著差异,表明三者的结构组成成分有一定差异。23个微粉样品的乳化活性和乳化稳定性随粒度级别的减小而显著增加(P0.01)。33个微粉样品的蛋白质体外消化率随粒度级别的减小而显著增加(P0.01)。4不同粒级带皮菜籽粕微粉样品的吸水性与吸油性受其结构组成物质不同和粒度的双重影响,与粒度的相关性不明显。