Animal Plant and Food Inspection Center, JSCIQ,,Animal Plant and Food Inspection Center, JSCIQ,输日动物源性（蜂产品）残留限量及检测技术,报告人：沈崇钰 2006年4月 北京,,Animal Plant and Food Inspection Center, JSCIQ,,Animal Plant and Food Inspection Center, JSCIQ,介绍内容,一、日本肯定列表与蜂产品出口,二、蜂产品中各类抗生素残留检测,,Animal Plant and Food Inspection Center, JSCIQ,,Animal Plant and Food Inspection Center, JSCIQ,一、日本肯定列表与蜂产品出口,,Animal Plant and Food Inspection Center, JSCIQ,,Animal Plant and Food Inspection Center, JSCIQ,2003年5月，日本修订了《食品卫生法》 依据新修订的《食品卫生法》，2006年5月29日，实施食品中农业化学品（农兽药及饲料添加剂）残留限量“肯定列表制度”,,Animal Plant and Food Inspection Center, JSCIQ,,Animal Plant and Food Inspection Center, JSCIQ,日本将要实施的“肯定列表制度”，对食品、农产品中所有农业化学品残留物都作了明确规定。
其中15种农药、兽药禁止使用；797种农药、兽药及饲料添加剂设定了53862个限量标准（包括“现行标准”和“暂定标准”）；对没有设定限量标准的，执行“一律标准”，即含量不得超过0.01毫克/公斤只有65种天然和化学合成物质（主要是营养剂）做为豁免物质不设限量从2006年5月29日起，只有符合“肯定列表制度”要求的食品、农产品才能进入日本市场Animal Plant and Food Inspection Center, JSCIQ,,Animal Plant and Food Inspection Center, JSCIQ,,日本厚生省网站上公布了一批检测方法（176个） 单品种检测方法166个 多残留检测方法6个 大多数为植物源性食品中农药残留检测方法 涉及肯定列表中505种化学物质,,Animal Plant and Food Inspection Center, JSCIQ,,Animal Plant and Food Inspection Center, JSCIQ,,这176个检测方法中涉及蜂蜜检测的很少 方法陈旧，很多方法都是上世纪80年代的 且大多数不适用（都是单残留检测方法） 日本国内实验室也不使用这些方法 日本国内大多采用多残留检测技术,,Animal Plant and Food Inspection Center, JSCIQ,,Animal Plant and Food Inspection Center, JSCIQ,,目前日本对蜂产品中残留分类,兽药类,,农药类,添加剂类,,极少,,,Animal Plant and Food Inspection Center, JSCIQ,目前日本对蜂产品中动物用药分类,,兽药分类,氯霉素类,四环素类,硝基呋喃类,氨基糖苷类,大环内酯类,Β内酰胺类,苯并咪唑类,硝基咪唑类,阿维菌素类,大环内脂类,同化激素类,苯乙胺类,,,,Animal Plant and Food Inspection Center, JSCIQ,,Animal Plant and Food Inspection Center, JSCIQ,,农药分类,菊酯类,有机氯类,有机磷类,其它,杀鼠剂类,,,,Animal Plant and Food Inspection Center, JSCIQ,,Animal Plant and Food Inspection Center, JSCIQ,出口日本蜂蜜现在要求检测的重要兽药项目（高风险项目） -（双氢）链霉素（氨基糖苷类） 氯霉素 硝基呋喃类 喹诺酮类 泰勒菌素、红霉素（大环内脂类） β内酰胺类,,Animal Plant and Food Inspection Center, JSCIQ,,Animal Plant and Food Inspection Center, JSCIQ,,二、蜂产品中各类抗生素残留检测技术 （高风险类药物）,,,Animal Plant and Food Inspection Center, JSCIQ,,Animal Plant and Food Inspection Center, JSCIQ,,氯霉素（Chloramphenicol, 简称CAP）是一种十分有效的广谱抗生素，自从1950年来，广泛的应用于食用动物的疾病的预防和治疗。
一、氯霉素检测,目前限量暂时定为0.1ug/kg,,Animal Plant and Food Inspection Center, JSCIQ,,Animal Plant and Food Inspection Center, JSCIQ,,至今为止，氯霉素残留仍然在蜂蜜和王浆产品中大量检出,,Animal Plant and Food Inspection Center, JSCIQ,,Animal Plant and Food Inspection Center, JSCIQ,,目前检测氯霉素的方法,,Animal Plant and Food Inspection Center, JSCIQ,,Animal Plant and Food Inspection Center, JSCIQ,,,目前为止，LC/MS/MS方法是最为普遍的确证方法,MS-MS,然而，有新的检测氯霉素技术出现,,Animal Plant and Food Inspection Center, JSCIQ,,Animal Plant and Food Inspection Center, JSCIQ,,推荐检测技术-生物传感检测 Biosensor technology,,Animal Plant and Food Inspection Center, JSCIQ,,Animal Plant and Food Inspection Center, JSCIQ,,蛋白捕获体核分析物之间特定作用 可以实时监控并定量分析(无需标记) 测定原理： Surface Plasmon Resonance (SPR) Immobilisation of binding partner 分析物通过微流体注射技术从分析物表面通过 传感器表面可以再生,简介: 生物技术,,Animal Plant and Food Inspection Center, JSCIQ,,Animal Plant and Food Inspection Center, JSCIQ,,Autosampler unit,Optical Detection Unit & IFC,Docking station,,,,,Remote data acquisition,,Sensor chip,,,Animal Plant and Food Inspection Center, JSCIQ,,Animal Plant and Food Inspection Center, JSCIQ,,Biosensor chip,,Animal Plant and Food Inspection Center, JSCIQ,,Animal Plant and Food Inspection Center, JSCIQ,,,,,,,Surface Plasmon Resonance (SPR) -1,,4. IFC – Flow channel,Reflected light,3. Sensor surface with gold film,,Polarized light,2. Prism,Optical Detection Unit,1. Light- source,,Sample,,1. Sample is loaded onto the chip,,Animal Plant and Food Inspection Center, JSCIQ,,Animal Plant and Food Inspection Center, JSCIQ,,,,,,,,4. Flow channel,Reflected light,3. Sensor surface with gold film,,Polarized light,2.Prism,Optical Detection Unit,1. Light- source,,,Sample,,2. Molecular binding detected,,Animal Plant and Food Inspection Center, JSCIQ,,Animal Plant and Food Inspection Center, JSCIQ,,,,,,,,,MASS CHANGE,TIME,,Flow channel,Reflected light,Sensor surface with gold film,,Polarized light,Prism,Light- source,Dissociation,Association,,,,Sample,,3. Molecular dissociation detected,Optical Detection Unit,,Animal Plant and Food Inspection Center, JSCIQ,,Animal Plant and Food Inspection Center, JSCIQ,,本实验室开发王浆和蜂蜜中氯霉素检测方法原则,1、准确,2、快速,3、节约成本,,,使用内标,不使用固相萃取,,Animal Plant and Food Inspection Center, JSCIQ,,Animal Plant and Food Inspection Center, JSCIQ,,,2、可以利用王浆中氯霉素的提取方法，结合试剂盒技术 进行初筛， 节省企业成本。
1、已有蜂蜜和王浆中氯霉素检测国标方法，,总结,3、生物传感检测技术在欧盟已经开始使用，测定氯霉素、甚至13种磺胺等，但是仪器昂贵，使用面相对质谱较窄,,Animal Plant and Food Inspection Center, JSCIQ,,Animal Plant and Food Inspection Center, JSCIQ,二、硝基呋喃类代谢物检测和非人为污染途径,,,,Animal Plant and Food Inspection Center, JSCIQ,,Animal Plant and Food Inspection Center, JSCIQ,高效液相色谱－质谱联用（唯一仪器方法）,优点：抗干扰能力强，定性准确，定量下限低，可以达到欧盟检测要求,缺点：仪器昂贵，操作复杂，需要衍生化,目前可以测定四种硝基呋喃类代谢物的方法,目前限量定为1ug/kg,,Animal Plant and Food Inspection Center, JSCIQ,,Animal Plant and Food Inspection Center, JSCIQ,是否会有其它污染途径（非人为因素）？,1、 Azodicarbonamide (ADA)－偶氮甲酰胺,2、卡拉胶,3、食品加工过程中氧化剂或者加热,,Animal Plant and Food Inspection Center, JSCIQ,,A。