【作者】 郭伟；

【导师】 张建新；

【作者基本信息】 西北农林科技大学 ， 食品科学， 2006， 硕士

【摘要】 磺胺类药物是一类广谱抗生素,由于其毒性,欧盟等许多国家要求动物源性食品中磺胺类药物残留量不得高于0.lmg/kg。国内外已经建立了多种检测方法,如气相色谱法、气质联用法、液相色谱法等,气相色谱和液相色谱法灵敏度低无法满足现在检测的需要。气质法灵敏度高,但需要衍生化,样品前处理复杂。因此,有必要建立一种有效的测定方法。本文对高效液相色谱法和液相色谱-大气压化学电离-质谱联用法测定磺胺类药物进行了比较。高效液相色谱法的检出限为20μg/kg,灵敏度低。液质联用设备的检出限是4μg/kg,灵敏度高,可以大大的提高检测的稳定性、准确性、重现性、检出限。对色谱条件和质谱参数进行了优化,相对标准偏差为1.3%～9.7%。比较了不同提取方法的提取效果,确定了样品匀浆2分钟后,在温度30℃,超声功率700W下超声120S的提取方法,提取液经oasis MCX小柱固相萃取净化,优化了洗脱液,讨论了有无固相萃取的影响;并对猪肉样品进行了3个水平加标回收试验,方法回收率在59.0%～124.5%之间,方法精密度1.4%～15.4%,方法检出限为3.87ng/g ~4.21ng/g。方法的灵敏度远低于欧盟最大残留量的要求,这个方法简单、准确,适于测定猪肉中的磺胺类药物。对市售的79份猪肉样品进行检测分析发现,阳性检出率为63.29%,磺胺类药物残留超标率为3.80%。各肉类组织磺胺类药物残留超标的情况集中于猪肾、猪肝,同时阳性率较高也集中于猪肾、猪肝。7种磺胺类药物中检出率最高的是SM,为53.16%,其次是SQX和SD,分别为11.39%和10.13%。残留超标的药物全部是SM,超标率是7.14%。这说明漯河市区猪肉中兽药污染问题较为严重。更多还原

【Abstract】 Sulfonamides(SAs) is a broad-spectrum antobiotic, Because of its toxic properties, it has been banned from producing animal foods in the European community etc. than 0.1mg/kg . Several analytical methods for the determination of SAs in different biological materials, based on gas chromatography , gas chromatography-mass spectrometry, liquid chromatography have been published. But GC and HPLC can not satisfied with analytical requirement because of low sensitivity. GC-MS method has demonstrated excellent sensitivity, but the sample treatment is time-consuming, require derivatization. Therefore, it is necessary to install an effective determination method.The method to determinate sulfonamides, HPLC was compared with LC-APCI-MS. HPLC method ,its detection limit is 20μg/kg, has low sensitivity. while LC-APCI-MS, its detection limit is 4μg/kg, has high sensitivity, can improve greatly stability、accuracy、reproducibility and detection limit. LC conditions and MS parameters are optimized, RSD is 1.3%～9.7%.The effects of different extraction method on rate were studied. The sample was homogenated 2 minutes , and ultrasonic 120s under the condition of 30℃and 700W. The extracted liquid was purified by oasis MCX , elution liquid was optimized, the effects of solid phase extraction on purity were studied. Recoveries were ranged from 59.0% to 124.5% for all compounds at three different spiked levels ,relative standard deviations(RSD) are between 1.4% and 15.4%, and the limits of detections ranged from 3.87 ng/g to 4.21ng/g. The sensitivity of this methods far below the maximum residue limit established by European Commolunity. This method is simple ,accurate and suitable for identification and quantification of sulfonamides in pork tissue.The sulfonamides residual level of 79 pork tissue sample bought from market were determined, results showed that positive rate was 63.29% and ultra-standard rate was 3.80%. pork kidney and pork liver were the most positive or ultra-standard tissue.SM , the highest positive rate sulfonamide of 7 sulfonamides, is 53.16%, followed by SQX and SD, is 11.39% and 10.13%, respectively. All the ultra-standard drug is SM, whose ultra-standard rate is 7.14%. it showed that the pollution of sulfonamides in pork tissue in Luohe urban is serious.更多还原