【作者】 薛晓锋；

【导师】 赵静；

【作者基本信息】 中国农业科学院 ， 农产品质量与食物安全， 2008， 硕士

【摘要】 蜂王浆是由哺育蜂头部咽下腺和上颚腺共同分泌的粘性物质,是蜂王幼虫正常发育的必需食物。蜂王浆作为保健和功能食品,具有多方面的功效,长期食用有益于人体健康。中国是蜂王浆的主要生产和出口国家,主要出口到欧洲,日本和美国。随着蜂王浆产品消费的增加,蜂王浆中的药物残留逐渐引起了人们的关注。此外,随着中国蜂王浆出口量的增加,欧盟,美国和日本等国为了保护本国的贸易利益,设置了许多技术壁垒。这些国家和组织制订了苛刻的药物残留限量,建立相应的检测方法来限制中国蜂王浆产品出口。常规的测定方法很难满足这些国家和组织的限量要求。目前,我国并没有相应的检测蜂王浆中四环素的标准方法。为了保证我国蜂王浆产品的正常出口,建立简单快速测定蜂王浆中的四环素类药物残留的方法是非常必要和有意义的。尽管已经报道了许多测定四环素类药物的方法,但这些方法并不适合测定蜂王浆中的四环素族残留,因为蜂王浆基质比其他食品更复杂,需要建立新的测定方法来监控蜂王浆中四环素族残留。在本研究中,我们制订了LC/MS法测定蜂王浆中的四环素残留。蜂王浆样品中的四环素药物残留用0.1mol/L Na2EDTA-Mcllvaine缓冲溶液提取,经过Oasis HLB柱净化,然后采用LC/MS进行测定。本方法的加标回收率在65.0%～86.8%之间,相对标准偏差在5.53%～11.30%之间,对蜂王浆中土霉素、四环素的检出限小于10 ng/g,金霉素、多烯环素的检出限小于20 ng/g。方法的各项指标符合兽药残留的要求。方法经过超高效液相色谱串联质谱的验证,证明方法有很好的适用性。方法经过不同实验室的复核,各项参数符合实验室间方法比对的各项要求,方法经过审定,形成相应的国家标准。应用本研究制订的标准方法对我国蜂王浆的主要生产区的一些王浆样品进行检测,抽检的样品中有四环素类药物检出,主要检出的药物为土霉素,金霉素,说明我国蜂王浆产品中四环素族残留存在潜在威胁。更多还原

【Abstract】 Royal jelly (RJ) is a viscous substance secreted by the hypopharyngeal and mandibular glands of nurse worker bees (Apis mellifera L.) that constitutes the essential food for the larvae of the queen bee.In modern diets, the use of RJ has significantly increased because of the trend toward use of healthy, organic, nutraceutical, and functional foods, and dietary supplements. The peoples’s republic of China is the world’s largest producer and exporter of royal jelly. Most of the Chinese RJ production is distributed in Europe, Japan, and the United States. As a result of the increasing interest in RJ in human health, the concern of drugs residues in royal jelly is also increasing. In addition, with export quantity of RJ continuously increasing, EU, USA and Japan made lots of TBs (technological barriers) in order to protect native trade benefits. Some tough MRL (maximum residue limit) and relative testing methods was established by EU, USA and Japan. It is difficult for common methods to analysis tetracyclines in RJ. Nowdays, there is no standard methods available for determination of tetracyclines in RJ in our country. Development of simple and rapid methods for determination of tetracyclines in RJ is therefore necessary and would be valuable for export trade of RJ.Although a number of methods have been reported for determination of tetracyclines in different tissues and products, these methods can not be suitable to monitoring tetracyclines in RJ because of the matrix of RJ is more complex than others’s. In this study, we developed a LC/MS method for determination of tetracyclines in RJ. Tetetracycline antibiotic residues were extracted from royal jelly samples using a buffer containing 0.1mol/L Na2EDTA-Mcllvaine.The sample extracts were further purified and enriched by Oasis HLB.The recoveries of four tetracyclines ranged from 65.0 to 86.8% in fortified blanks, the relative standard deviations were between 5.53 % and 11.30 %. The method detection limits of oxytetracycline and teracycline were <10μg/kg, chlortetracycline and doxycycline were <20μg/kg, respectively. These results indicated the method meet the demand of animal drugs residue analysis. The developed method was validated by ultra-performance liquid-MS-MS and other laboratories. After examination the method developed national determination method standard.Some samples collected from the main RJ produce areas were detected using the developed method. Some positive samples were found among which oxytetracycline and chlortracycline were main detectable drugs, which means it has a potential threat in RJ consumption.更多还原