高效液相色谱紫外电化学串联检测生物样品中克仑特罗残留

采用高效液相色谱紫外电化学串联法测定了动物性组织和体液中克仑特罗残留的含量。样品经初提 ,液液萃取 ,弱阳离子交换柱分离富集浓缩后经高效液相色谱分离 ,紫外电化学检测器串联检测。液相色谱的流动相为甲醇 :0 0 1mol LKCl溶液 (4 5 :5 5 )。色谱柱为HypersilBDSC18柱。紫外检测波长 2 4 4nm ,电化学采取脉冲方式 ,峰电压 1 0V。克仑特罗浓度与紫外及电化学响应信号均呈良好的线性关系。不同加标水平的回收率在 4 2 2 %～ 96 1%之间。样品的定量限为 0 5 μg kg。对猪肉、猪肝、猪肾、鸡肉和尿液、血液等生物样品进行了测定 ,测定结果满意     

Determination of nitrofuran metabolites residues in animal tissues by LC-MS/MS method

A LC-MS-MS method is presented to analyze simultaneously the metabolites of four nitrofuran veterinary drugs in animal muscle tissue e.g., furazolidone, furaltadone, nitofurantoina and nitrofurazone. The sample clean up were performed by a liquid-liquid extraction with ethyl acetate, after a hydrolysis and derivatization with 2-nitrobenzaldehyde. Nitrofurane metabolites were determined by LC-ESI-MS/MS in positive mode. The LC was equipped with column Luna C18 Phenomenex. A binary gradient mobile phase was used as methanol solvent B containing 0.5 mM ammonium acetate and methanol (80:20 v/v). The method was validated according to criteria of Decision Commission No 2002/657/EC. Samples were fortified with metabolites of nitrofuran between 0.5-2.0 microg/kg with AOZ-d4, and AMOZ-d5 as internal standard. The mean recoveries from meat spiked at 1.0 microg/kg were 84.5-109.7%. Limit of decision (CCalpha) was between 0.25-0.57 and capability of detection (CCbeta) 0.32-0.77 microg/kg.     

抗玉米赤霉烯酮单克隆抗体免疫亲和柱的研究制备

目的研究制备抗玉米赤霉烯酮（Zearalenone,ZEN）单克隆抗体免疫亲和柱（IAC）。方法用辛酸硫酸铵法纯化抗ZEN单克隆抗体,将纯化好的单抗与溴化氰活化的4FF葡聚糖偶联制备抗ZEN单克隆抗体免疫亲合柱。采用紫外扫描鉴定偶联反应,间接竞争酶联免疫吸附法及高效液相色谱法（HPLC）对制备好的免疫亲合柱进行评价。结果每根抗ZEN单克隆抗体免疫亲和柱,使用0．5ml溴化氰活化的4FF葡聚糖,350ugZEN单克隆抗体,柱容量为0．40ug。小麦样品添加ZEN标品60—300ug／kg,回收率76．33％-90．10％,相对标准偏差6．68％-10．93％。使用本实验室制备的抗ZEN单克隆抗体免疫亲合柱建立了IAC．HPLC方法,并检测小麦、玉米、饲料样品30份,结果有17份样品为阳性,阳性率56．67％,样品中ZEN含量为31．33～377．84ug／kg;信噪比为3：1时,检测下限为10．00ug／kg。结论抗ZEN单克隆抗体免疫亲和柱能快速特异地将ZEN从样品中分离出来,并同时完成净化和浓缩步骤,是一种简便的净化方法。     

Optimization of analytical methods for assay of ochratoxin A in the foodstuffs

Ochratoxin A is a mycotoxin produced by widespread mold fungi of the genera Aspergillius and Penicillium. It is a common contaminant of cereals, coffee, wine, dried fruits, and spicery. There is evidence that ochratoxin A has nephrotoxic, immunosuppressive, embryotoxic, teratogenic, and carcinogenic effects on many species of mammals. Its maximum allowable concentration established by the Alimentarius Code and the European Union is 5 microg/kg for cereals and 3 microg/kg for ready-made cereals. Two optimized techniques (silica gel column chromatography (CC) or immunoaffinity CC for extract purification and high performance liquid chromatography with fluorescence detection) are proposed for the detection, identification, and assay of ochratoxin A in food commodities. The detection limit was 0.05 and 0.5 microg/kg, respectively. The developed techniques were used to assay the content of ochratoxin A in 46 samples of the grain gathered in different regions of Russia. Nine samples were contaminated by ochratoxin A at concentrations of 0.05 to 5 microg/kg.     

Determination of benzo[a]pyrene in charcoal grilled meat samples by HPLC with fluorescence detection

In this study, an HPLC procedure for the quantitative determination of benzo[a]pyrene (BaP) in charcoal grilled meat samples has been applied to the analysis of the Turkish meat samples. The grilled meat samples were first treated in alkaline medium, then BaP was extracted into n-hexane phase, purified on XAD-2 column and eluted with n-hexane/dichloromethane mixture (9:1,v/v). Separation and quantitative determination of BaP has been carried out by a C18 reversed phase column mounted HPLC with a fluorescence detection of 254-355 nm (excitation-emission). The BaP levels determined in grilled and over-grilled lamb and beef meats were 43.80 +/- 1.80 microg/kg, 31.33 +/- 0.94 microg/kg and 62.60 +/- 3.72 microg/kg, 37.60 +/- 3.84 microg/kg, respectively.     

用高压液相色谱法检测罐装食品中类雌激素双酚A和烷基酚

目的 建立不同基质食品中双酚A（BPA）、壬基酚（NP）和辛基酚（OP）等类雌激素的高压液相色谱法（HPLC）,检测市售罐装食品中类雌激素。方法 固体样品经甲醇超声提取、二氯甲烷萃取、浓缩。液体样品的分析采用NH。柱浓缩、富集和净化。HPLC采用WatersXTerra^TM MSC18液相色谱柱分离,甲醇．水作为流动相梯度洗脱。采用荧光检测,激发波长：225nm;发射波长：310nm。结果 建立的方法具有良好的线性关系,蔬菜类罐装食品和方便面中BPA、NP和OP的检出限分别为0．5、0．1和0．1μg/kg,鱼、肉类罐装食品BPA、NP和OP的检出限分别为1、0．5和0．5μg/kg。BPA、NP和OP加标回收率分别为74．9％～95．1％、76．3％～103．6％和72．1％～109．2％;相对标准偏差（RSD）分别为4．98％～11．2％、2．35％～8．88％和5．61％～12．3％。结论 该方法测定罐装食品及方便面中类雌激素（BPA、OP和NP）,具有较高的灵敏度和选择性,结果准确可靠、重现性好。     

市售腊肠中总亚硝基化合物检测

目的建立腊肠总亚硝基化合物(TNOC)测定方法,调查腊肠中TNOC污染情况。方法在以往液体标本测定方法的基础上建立腊肠TNOC的化学裂解-热能分析仪测定方法,该法具有区分热和酸不稳定物质的优点。随机采集市售腊肠32份,采用化学裂解-热能分析仪法测定腊肠中总亚硝基化合物含量。结果研究发现,AG1-X8阴离子树脂可以有效去除样品中硝酸盐的干扰,又不影响亚硝基化合物的测定;0.2%HCl/HAc既能很好裂解NaNO2,又不会使不稳定的亚硝酰胺大量分解;样品加标平均回收率为86%(83%~89%);TNOC检出限为6.6μg(N-NO)/kg,相对标准差为5.9%。32份腊肠样品中TNOC检出率为93.8%;平均含量为49.09μg/kg(95%CI39.15~126.35μg/kg)。结论该方法具有准确性和可重复性。腊肠中TNOC污染较普遍,应当加强这方面的食品卫生监督。     

PXC和EMR-Lipid QuEChERs技术在动物源性食品中多种β-受体激动剂残留检测的前处理效果对比

目的 比较PXC和EMR-Lipid QuEChERs(简称EMR-L)萃取法对动物源性食品中多种β-受体激动剂残留检测效果的影响.方法 利用UPLC-MS/MS分析技术,使用PXC固相萃取小柱和EMR-Lipid QuEChER两种前处理材料,对相同样品的检测结果进行对比和分析.结果 两种前处理方法在0.5～10 n...     

同位素标记-超高效液相色谱-串联质谱法快速检测肉类中20种β受体阻断剂

目的 建立肉类(猪、羊、牛肉)中20种β受体阻断剂的同位素标记-超高效液相色谱-串联质谱快速检测方法。方法 样品经三氯乙酸酸解提取后,经Agilent Captiva EMR-Lipid柱净化,再经Waters BEH C₁₈色谱柱分离,ESI源正离子模式进行多反应监测(MRM),内标法定量。结果 20种β受体阻断剂线性范围为0.5～20 μg/L,相关系数大于0.996,检出限为0.01～0.10 μg/kg,定量限为0.03～0.30 μg/kg。3个加标水平(1.0 μg/kg、5.0 μg/kg、10 μg/kg)的回收率在80.3%～118.7%之间,相对标准偏差为3.2%～17.2%。结论 该方法前处理简单、快速、准确、灵敏度高,适用于肉类食品中β受体阻断剂的定性、定量检测。     

加速溶剂萃取/凝胶渗透色谱净化-气质联用法测定烟熏腊肉中24种多环芳烃

目的 建立烟熏腊肉中24种多环芳烃的气相色谱-质谱联用快速检测方法。方法 腊肉样品与硅藻土充分混合后置于萃取池中加速溶剂萃取,萃取液经过凝胶渗透色谱(GPC)去除油脂,SPE硅胶柱去除极性组分,经DB-EUPAH色谱柱分离后,质谱检测,内标法定量。结果 24种PAHs的线性范围为 1.0～300ng/ml,线性相关系数r为0.9975～0.9999。方法检出限在0.5～5.0μg/kg之间,加标回收率为70.4%～118.5%,相对标准偏差为5.43%～9.74%(n=3)。结论 该方法准确度高,重现性好,适合于烟熏肉中24种PAHs的同时测定。     

Immunoaffinity columns and determination of ochratoxin A in cereals by HPLC. Part I.: Evaluation of extraction using methanol/water

The method for ochratoxin A determination in cereals (wheat, rye) was described. Application of immunoaffinity columns (IAC) for clean-up of extracts was investigated. The ochratoxin A content was determined by high-performance liquid chromatography using C18 column and fluorimetric detection at 330 nm (excitation) and 460 nm (emission). The mean recovery of ochratoxin A was 65-78%. The limits of detection (LOD) and quantification (LOQ) were 0.015 and 0.025 microg/kg, respectively. The positive results were confirmed by reaction with BF3 complex in methanol.     

Determination of chloramphenicol residues in milk powder using molecular imprinted polymers (MIP) by LC-MS/MS

The method is presented to analyze chloramphenicol in milk powder. Sample was clean-up by used molecular imprinted polymers (MIP). The determination was performed by LC-ESI-MS/MS. The LC was equipped with column Luna C18 Phenomenex. CAP-d5 was used as internal standards. The method was validation according to the criteria of Decision Commission No 2002/657/EC. Recoveries for the level 0.3 microg/kg was in the range 104-111%. The limit of decision (CCalpha) and detection capability (CCbeta) was respectively 0.06 microg/kg and 0.09 microg/kg.     

Studies and safety evaluation of aflatoxins in herbal plants

Herbs and herbal products are commonly used in food and pharmaceutical industries. The aim of this study was to test herbal plants for contamination with aflatoxins (AF), genotoxic, cancerogenic and hepatotoxic compounds which can cause immunotoxic and allergic effects as well as growth disorders. Aflatoxins were determined by high performance liquid chromatography (HPLC) with post column derivatization involving bromination with pyridinium hydrobromide perbromide (PBPB). Extracts was cleaned-up by immunoaffinity columns (IAC). The contents of aflatoxins B, B, G, and G, in more than 500 herbal plants samples mainly from Eastern Poland were investigated. Samples were supplied by manufacturers (herbal facilities) in 2006-2010 years. In all the evaluated samples the levels of aflatoxins above the detection limits of methods applied were not observed: for AF B1--0.2 microg/kg; AF B2--0.03 microg/kg; AF G1--0.3 microg/kg; AF G2--0.03 microg/kg (PN-EN 14123) and for AF B1--0.15 microg/kg (Ph. Eur.6, 2008:2.8.18). All the herbal plants tested for contamination with aflatoxins should be considered safe, which indicates that manufacturers used good manufacturing practices during drying and storage of raw materials.     

气相色谱-串联质谱法测定滩涂生物样本中的六六六和滴滴涕

目的建立滩涂生物样本中的六六六(HCHs)和滴滴涕(DDTs)的气相色谱-串联质谱(GC-MS/MS)测定法。方法取可食部位匀浆样品加无水硫酸钠脱水、使用石油醚进行超声萃取,再加硫酸磺化后静置取有机相氮气吹干定容,取上清液经HP-5MS Ultra Inert毛细管气相色谱柱(30 m×250μm,0.25μm)分离,气相色谱-串联质谱分离检测,外标法定量。结果本法六六六和滴滴涕在0.100μg/L^10.0μg/L线性相关系数均≥0.999,方法检出限均为0.02μg/kg,平均样本加标回收率为57.6%~100%,相对标准偏差(RSD)在0.100μg/kg水平为15.1%~23.0%,1.00μg/kg水平为8.12%~17.1%,10.0μg/kg水平为3.22%~9.03%。使用本方法检测实际样品,六六六检出率为44.0%,滴滴涕检出率为99.0%,检出浓度为0.035μg/kg^8.17μg/kg。结论该方法前处理过程简便,定性及定量准确,灵敏度高,满足批量样品的检测。     

Optimization of determination of aflatoxins in foods with bromine postcolumn derivatization

The method for determination of aflatoxin B1, B2, G1 i G2 in nuts, culinary spices, cereals and cereal products was described. To optimize the analytical procedure in several products, condition of proper extraction, clean-up, HPLC and detection were selected. After extraction by means of methanol and water (80+20 v/v) or (70+30 v/v), clean-up on IAC columns, HPLC on C18 columns--Nucleosil and Nova Pak with mobile phase-methanol, acetonitrile, water (20+20+60 v/v) was performed. For fluorometric detection at 362/430 nm, post-column derivatization of aflatoxin B1 and G1 with bromine was carried out. The mean recovery of the method depending on matrix and aflatoxin, was 52-102% at RSD% 0.2-8.3. LOD and LOQ, respectively were: 0.01 and 0.02 microg/kg for nuts and 0.05 and 0.1 microg/kg for culinary spices and cereal products. The concentrations of aflatoxins in 86 samples of foods from market were below the permissible maximum levels legally binding.     

DAD-FLD串联SPE-HPLC测定肉制品中沙丁胺醇、莱克多巴胺和克仑特罗

目的:建立一种高效液相色谱法同时测定肉制品中沙丁胺醇、莱克多巴胺和克仑特罗的色谱分离条件和前处理方法。方法:采用HLB固相萃取小柱对样品进行提纯和富集,反相C18柱进行分离,流动相为CH3OH∶NaH2PO4(0.1%甲酸)(40∶60),流速0.8 ml/min,DAD检测波长为243 nm,荧光检测激发波长为226 nm,发射波长为306 nm。结果:用本方法检测,能很好的分离三种物质。本方法相关系数可达0.999,相对标准偏差为0.75%～2.01%,回收率在90%～110%之间。结论:本法可同时测定肉制品中的沙丁胺醇、莱克多巴胺和克仑特罗,结果准确、灵敏度高,环境污染小。     

QuEChERS - 超高效液相色谱串联质谱法测定果蔬中33种农药残留

目的 基于QuEChERS技术,采用超高效液相色谱串联质谱（UPLC - MS/MS）建立了水果和蔬菜中杀虫剂、杀菌剂等33种农药残留的检测方法。方法 样品用乙腈提取,经无水硫酸镁、N - 丙基乙二胺（PSA）和石墨化碳黑（GCB）净化,BEH C18色谱柱分离,以正离子多反应监测模式、外标法定量。结果 33种农药在0.5～100 ng/ml范围内具有良好的线性关系,相关系数均大于0.999,定量限和检出限分别为0.5～2.0 μg/kg和0.2～0.6 μg/kg。低、中、高3个加标水平下,33种农药的回收率在79.2%～119.3%之间,相对标准偏差为0.1%～9.7%。应用建立的方法对75份果蔬样品进行检测,检出15种农药,检出率4.0%～14.6%,含量为0.008 52～7.80 mg/kg。结论 本法操作简便、灵敏、准确,适用于果蔬中多种农药残留的快速检测。     

A modified routine analysis of arsenic content in drinking-water in Bangladesh by hydride generation-atomic absorption spectrophotometry

The high prevalence of elevated levels of arsenic in drinking-water in many countries, including Bangladesh, has necessitated the development of reliable and rapid methods for the determination of a wide range of arsenic concentrations in water. A simple hydride generation-atomic absorption spectrometry (HG-AAS) method for the determination of arsenic in the range of microg/L to mg/L concentrations in water is reported here. The method showed linearity over concentrations ranging from 1 to 30 microg/L, but requires dilution of samples with higher concentrations. The detection limit ranged from 0.3 to 0.5 microg/L. Evaluation of the method, using internal quality-control (QC) samples (pooled water samples) and spiked internal QC samples throughout the study, and Standard Reference Material in certain lots, showed good accuracy and precision. Analysis of duplicate water samples at another laboratory also showed good agreement. In total, 13,286 tubewell water samples from Matlab, a rural area in Bangladesh, were analyzed. Thirty-seven percent of the water samples had concentrations below 50 microg/L, 29% below the WHO guideline value of 10 microg/L, and 17% below 1 microg/L. The HG-AAS was found to be a precise, sensitive, and reasonably fast and simple method for analysis of arsenic concentrations in water samples.     

凝胶渗透色谱-气相色谱-串联质谱法测定血清中7种多氯联苯残留量

目的:建立了人血清样品中7种多氯联苯残留量的分析方法。方法:样品以丙酮-正己烷(1+2,V/V)为提取溶剂,经高速匀浆方法提取,提取液经凝胶渗透色谱净化,除去样品中大部分的血糖和蛋白等干扰基质,采用VF-5ms(30 m×0.25 mm×0.25μm)色谱柱对7种多氯联苯进行分离,通过多反应离子监测模式扫描检测,有效地降低了样品中的复杂基质所带来的背景干扰。采用色谱保留时间和质谱碎片离子丰度比定性,外标法定量。结果:方法的相关系数r>0.999,最小检出限为0.5μg/kg～1.0μg/kg。在3种浓度添加水平5.0μg/kg、10.0μg/kg、20.0μg/kg下,其平均回收率为87.6%～101%,相对标准偏差为2.5%～10.3%(n=6)。结论:实验证明,该方法是一种快速、准确、灵敏度高的检测血清样品中多氯联苯残留量的检测方法。     

2014—2019年济南市市售畜肉中β-受体激动剂含量调查

目的 监测济南市市售畜肉中β-受体激动剂含量,为食品行业监管和暴露风险评估提供依据。方法 2014—2019年,在济南市采集不同市场来源的畜肉及内脏,用固相萃取-超高效液相色谱串联质谱法检测其中的克伦特罗、莱克多巴胺、沙丁胺醇、特布他林,并分析残留水平。结果 六年共检测畜肉397份,β-受体激动剂检出率20.15%(80/397),其中克伦特罗检出率最高为15.62%(62/397)。采自农贸市场的畜肉中β-受体激动剂检出率明显高于采自超市的样品(P<0.01),羊、牛类样品中β-受体激动剂检出率明显高于猪类样品(P<0.05),内脏样品中的检出率明显高于肌肉(P<0.05)。结论 济南市畜肉中克伦特罗检出较多,牛、羊养殖、屠宰、销售等环节的监管需要加强,牛、羊肉特别是内脏中β-受体激动剂暴露风险较高。