共查询到17条相似文献,搜索用时 93 毫秒
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采用HPLC测定猪肉中磺胺类药物的残留,以Cloversil C18色谱柱,甲醇-1%乙酸水溶液作为流动相进行梯度洗脱.柱温30℃,进样量5 μ L,流速0.6 mL/min,240-280 nm波长紫外检测.经测定,猪肉中含有磺胺嘧啶、磺胺甲基异唑、磺胺噻唑、磺胺二甲嘧啶和磺胺喹啉等磺胺类物质.从而建立了一种快速、准确测定猪肉中磺胺类药物残留量的检测方法. 相似文献
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以微生物显色为原理,建立一种对畜禽肉中单一或配伍使用的抗生素进行联合初筛的高通量方法,并用色谱法对阳性样品进行验证。以大肠埃希氏菌(Escherichia coli,CICC 23657)作为指示菌,选取适当的抗生素残留提取方法,并通过单因素试验优化检测液配方及检测体系组成,最终实现对不同类别抗生素的联合检测。结果表明:选取柠檬酸-丙酮缓冲液进行提取,提取效率达到86%~88%,相对标准偏差为3.9%~4.3%;蛋白胨添加量为1.0 g/100 mL、溴甲酚紫指示剂添加量为2.0 mg/100 mL、pH值为7.2时,检测液显色效果较好;菌悬液初始吸光度(A600 nm)为0.4,检测液、菌液、样品提取液体积为150 μL∶50 μL∶100 μL时,检测效果最佳,对畜禽肉中喹诺酮类抗生素的检出限为60~180 μg/kg,氨基糖苷类检出限为60~140 μg/kg,喹诺酮类与氨基糖苷类配伍使用时的检出限为40~180 μg/kg;进一步用色谱法对50 份样品的初筛结果进行验证,无假阴性样品存在,说明该方法可用于畜禽肉中抗生素残留的初筛。 相似文献
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高通量微生物显色法快速检测动物源性食品中抗生素残留 总被引:2,自引:0,他引:2
建立一种采用高通量微生物显色法对动物源性食品中抗生素残留进行筛检,再结合高效液相色谱-串联质谱(high performance liquid chromatography-tandem mass spectrometry,HPLC-MS/MS)法对阳性样品进行复测的分析检验方法。本方法利用嗜热脂肪芽孢杆菌(Bacillus sterothermophilus)作为指示菌,制备96微孔板,可同时对不同类别多种抗生素进行联合检测。结果表明:该微生物显色法操作简便、快捷,成本低,结果准确且易判断,选取pH 7.4磷酸盐缓冲液进行提取,以反应液150μL、菌液50μL(初始OD_(600 nm)为0.4左右)、样品提取液100μL作为检测体系,检测效果最佳,对动物源性食品中氨基糖苷类检出限为60μg/kg,β-内酰胺类检出限为20~40μg/kg,大环内酯类检出限为60~80μg/kg,四环素类检出限为40~60μg/kg,符合国内外对抗生素残留限量的要求。对60份动物源性样品进行检测,其结果与HPLC-MS/MS复测结果一致,说明该微生物法稳定性良好,可用于动物源性食品中抗生素残留的初筛检测。 相似文献
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目的:探究鲜乳中抗生素残留微生物检测方法。方法:采用利普斯50(E50)试剂盒、国家标准GB/T 4789.27—2008中嗜热链球菌抑制法(传统TTC法)和嗜热脂肪芽胞杆菌抑制法检测鲜乳中抗生素残留,并进行对比,以青霉素G钾盐为标准品加标检测。结果:61批牛奶样品的抗生素残留检测结果均为阴性,3种微生物检测方法抗生素残留最低检测限为0.005 μg·mL-1,检测结果一致。结论:利普斯50(E50)方法操作简单方便,检测量大,效率高,可作为鲜乳中抗生素残留检测首选方法,值得在奶牛养殖场、鲜乳制品企业和检验机构中推广应用。 相似文献
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LC-APCI-MS同时检测猪肉中7种磺胺类药物残留 总被引:2,自引:0,他引:2
为检测猪肉中磺胺类药物残留,建立了猪肉中7种磺胺类药物残留的LC—APCI—MS同时测定方法;样品经过匀浆、酸性甲醇超声波提取、柱净化后进行液相色谱-大气压化学电离-质谱分析;采用Zorbax XDB C18色谱柱,以均含0.2%乙酸的水和甲醇为流动相进行梯度洗脱,外标法定量;7种磺胺类药物的加标回收率为61,0%~114.7%(添加水平为1μg/kg,5pg/kg,10μg/kg),方法精密度1.5%~15.3%,方法检出限为3.92μg/kg~4.20μg/kg。 相似文献
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M.C. Bermúdez-Almada M.G. Pérez-Tello A.I. Valenzuela-Quintanar L. Vázquez-Moreno 《Journal of food science》1999,64(4):638-640
The residue depletion of oxytetracycline (OTC) from muscle tissue of cultured shrimp (Penaeus vannamei) was evaluated. OTC was measured using high performance liquid chromatography (HPLC) and a microbial receptor assay. Samples were taken on days 7, 14 and 21 during the treatment and 23, 25 and 28 after the treatment. OTC was detectable in all groups after 7 days depletion time at concentrations of 0.28, 0.19 and 0.05 μg/g for diets containing 500, 250 and 100 mg/kg OTC, respectively. Results by the microbial receptor assay were in good agreement with those by HPLC. 相似文献
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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 总被引:2,自引:0,他引:2
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。 相似文献
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S. R. Dognon G. Degand C. Douny P. Delahaut A. Igout M. Dahouda A. K. I. Youssao M. L. Scippo 《Food Analytical Methods》2018,11(12):3406-3416
In Benin, veterinary antibiotics are widely used for cattle breeding. This livestock contributes to 57% of the locally produced meat. The aim of this study was to assess the impact of the large use of antibiotics by determining the contamination level with antibiotic residues in bovine meat, in North Benin. Kidney and muscle samples taken from 50 bovine carcasses in the 2 main slaughterhouses of Parakou were analyzed for the presence of antibiotic residues by a screening method modified from the “New Two Plates Test” (NTPT), to identify tetracyclines, sulfonamides, and beta-lactam groups of antibiotics. Thirteen kidney and muscle samples were subjected to liquid chromatography coupled to tandem mass spectrometry analysis for the confirmation of tetracycline and sulfonamide residues. After modified NTPT screening, tetracycline residues were identified in 54% of cattle carcasses while beta-lactam and sulfonamide residues were present, respectively, in 2 and 6% of sampled animals. The LC-MS/MS analysis confirmed the presence in the kidney tissue of oxytetracycline, epi-oxytetracycline, tetracycline, and epi-tetracycline at maximum levels, respectively, of 1380, 350, 190, and 230 μg kg?1. Sulfamethazine residues were confirmed in one of cattle carcass at very high levels of 3900 μg kg?1 in kidney and 2220 μg kg?1 in muscle. Antibiotic residue levels were found above the maximum residue limit applied in the European legislation in 38% of the carcasses subjected to the LC-MS/MS analysis. These high levels of contamination with antibiotic residues are a potential threat for the health of consumers, and are of concern regarding the selection of antibiotic-resistant bacteria in animals and humans. 相似文献
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牛奶中多种磺胺类抗生素残留的HPLC快速分析 总被引:1,自引:0,他引:1
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。 相似文献