【摘要】：目的:我國(guó)作為抗生素的生產(chǎn)大國(guó),四環(huán)素類抗生素藥物的濫用、不合理應(yīng)用現(xiàn)象比較普遍。由此造成的細(xì)菌耐藥、畜產(chǎn)品藥物殘留、過(guò)敏中毒反應(yīng)等危害日益明顯,已直接威脅到人類的健康與安全。本文旨在建立可同時(shí)測(cè)定四環(huán)素(TC)、土霉素(OTC)、金霉素(CTC)和甲烯土霉素(MTC)四種類抗生素殘留的HPLC-CL檢測(cè)新方法,并對(duì)其在食品安全中的應(yīng)用進(jìn)行研究。方法:在最優(yōu)的反應(yīng)條件下用HPLC-CL聯(lián)用法測(cè)定四環(huán)素類抗生素。待測(cè)的四環(huán)素類樣品通過(guò)手動(dòng)進(jìn)樣器進(jìn)入高效液相系統(tǒng),流動(dòng)相為3.5×10-3mol/L甲烷磺酸(CH4O3S)的乙腈-水(20:80,v:v)溶液,流速為0.85ml/min,柱溫30℃,檢測(cè)波長(zhǎng)270nm,在C18分離柱上進(jìn)行等度洗脫分離,經(jīng)UV檢測(cè)器分離定性。柱后流出液首先與MCLA溶液混合,接著與Ce(Ⅳ)溶液混合。最后在化學(xué)發(fā)光檢測(cè)儀的流通池中產(chǎn)生化學(xué)發(fā)光信號(hào),由光電倍增管將其轉(zhuǎn)換成電信號(hào),并由工作電腦記錄發(fā)光信號(hào)強(qiáng)度。結(jié)果:四環(huán)素(TC)、土霉素(OTC)、金霉素(CTC)和甲烯土霉素(MTC)檢出限分別為2.5×10-9 mol/L,4.1×10-9 mol/L,1.0×10-8 mol/L,4.5×10-9 mol/L,它們的相對(duì)標(biāo)準(zhǔn)偏差為3.54%-8.76%(n=7)。經(jīng)實(shí)際樣品檢測(cè),得出豬肉的回收率為84.85%-111.0%,RSD為3.85%-10.87%,牛奶的加標(biāo)回收率為76.49%-115.7%,RSD為4.17%-10.70%。結(jié)論:本文建立了一個(gè)快速測(cè)定食品中四環(huán)素類抗生素殘留的HPLC-CL新方法。與其他體系相比,洗脫方式簡(jiǎn)單,簡(jiǎn)化了流動(dòng)相;與HPLC-UV相比,提高了選擇性,解決柱后流出物的干擾問(wèn)題;與HPLC-MS/MS相比,降低了檢測(cè)成本;最后,明確了發(fā)光機(jī)理,為化學(xué)發(fā)光技術(shù)的發(fā)展提供了理論依據(jù)。通過(guò)實(shí)際樣品檢測(cè),表明該方法在實(shí)際檢測(cè)中操作簡(jiǎn)便、分析快速,選擇性好、靈敏度高、回收率高,具有十分廣闊的應(yīng)用前景。
[Abstract]:Objective: as a large country producing antibiotics, the abuse of tetracycline antibiotics is common. Bacterial resistance, drug residues in animal products, allergic poisoning and other hazards are becoming more and more obvious, which have directly threatened the health and safety of human beings. A new HPLC-CL method for simultaneous determination of tetracycline (TC), oxytetracycline (OTC), chlortetracycline (CTC) and methylene oxytetracycline (MTC) was established and its application in food safety was studied. Methods: tetracycline antibiotics were determined by HPLC-CL under optimal reaction conditions. The tetracycline samples to be tested entered the high performance liquid phase system through a manual sampler. The mobile phase was a 3.5 脳 10-3mol/L methane sulfonic acid (CH4O3S) acetonitrile-water (20: 80 v: v) solution with a flow rate of 0.85 ml / min, column temperature of 30 鈩，

本文編號(hào)：2152763