【摘要】：磺胺類藥物(Sulfonamides,SAs)是指擁有對氨基苯磺酰胺結(jié)構(gòu)的一類藥物的總稱[1]。該類藥物因抗菌效果好、價格低廉等特點,使其在養(yǎng)殖領(lǐng)域得到廣泛應(yīng)用。但因一些不規(guī)范添加及使用,磺胺類藥物會在動物體內(nèi)殘留,食用這些超標的食物后,會引起人體的過敏反應(yīng)、毒性反應(yīng),產(chǎn)生抗藥性、引起“三致”(致畸、致癌和致突變)作用等。因此,從食品安全角度出發(fā),對動物源性食品中磺胺類藥物殘留量檢測問題一直較為關(guān)注。動物源性食品中磺胺類藥物殘留量的檢測方法一直在不斷更新和提高中,液質(zhì)聯(lián)用技術(shù)因為其選擇性、靈敏度、分析效能等方面的優(yōu)勢,是目前最常用的檢測方法,但其在實際檢測應(yīng)用中,常使用到三氯甲烷、丙酮等有機溶劑,如果操作不當(dāng),將會對實驗人員的身體操成傷害;而且大量使用有機溶劑也會大大增加檢測成本,對環(huán)境會有一定的破壞。本研究運用液質(zhì)聯(lián)用改進技術(shù),旨在減少有機溶劑的使用,減少實驗成本,提高檢測效率。重點研究并確定了五種提取溶劑(5%甲酸乙腈、5%乙酸乙腈、乙腈、三氯甲烷、乙酸乙酯),7種提取時間(0min、5min、10min、15min、20min、25min、30min),5個濃縮溫度(30℃、40℃、50℃、60℃、70℃),4種色譜柱(AQ5μm 2.1mmI.D.×150mm柱、Agilent ZORBAX Eclipse XDB-C_(18) 2.1×50mm柱、C_(18)-MGⅢ(pH 2-10)3μm 2.0mmI.D.×150mm柱、Waters ACQUITY UPLC HSS T3 1.8μm 3.0×50mm柱)對實驗結(jié)果的影響。本試驗確定了用于16種動物源性食品磺胺殘留的檢測方法,檢測結(jié)果顯示:16種磺胺在1~50μg/L范圍內(nèi)的線性相關(guān)系數(shù)(R2)為0.9965~0.9994,16種磺胺的加標回收率為85.82~109.51%,相對偏差為2.30~11.25%,檢出限為0.003~0.022μg/kg,定量限為0.2~1.1μg/kg。具體操作和檢測過程如下:樣品采用5%乙酸乙腈作為提取溶劑,提取20min,采用Bond ElutQuechers EM提取鹽、EMR-Lipidstp和EMR-polish管簡便、無毒的方法,對樣品進行凈化。在50℃的條件下用氮吹濃縮,采用C_(18)-MGⅢ(pH 2-10)3μm 2.0mmI.D.×150mm柱作為本試驗的色譜柱。通過與國標法(GB/T 20759-2006)檢測結(jié)果進行對比,相對偏差在4.28-9.76%之間。本測準方法準確率高,且有機溶劑用量較少,成本低,效率高,適用于動物源性食品中磺胺類藥物殘留的檢測。
[Abstract]:Sulfonamides (Sulfonamides,SAs) refer to a class of drugs with the structure of p-aminobenzenesulfonamide [1]. Because of its good antibacterial effect and low price, this kind of medicine has been widely used in the field of aquaculture. However, because of the addition and use of some non-standard drugs, sulfonamides will remain in animals. After eating these foods in excess of the standard, they will cause allergic reactions, toxic reactions, drug resistance and "teratogenicity" in the human body. Carcinogenesis and mutagenicity, etc. Therefore, from the point of view of food safety, the detection of sulfanilamide residues in animal-derived foods has been concerned. The methods for the detection of sulfanilamide residues in animal-derived foods are constantly being updated and improved. The liquid-mass spectrometry technology is the most commonly used detection method because of its advantages in selectivity, sensitivity, analytical effectiveness, etc. However, in the practical application, often used in trichloromethane, acetone and other organic solvents, if not properly operated, will be harmful to the body of the experimenter; And the large use of organic solvents will greatly increase the cost of detection, will damage the environment. The purpose of this study is to reduce the use of organic solvents, reduce the cost of experiments and improve the efficiency of detection. Five extraction solvents (5% acetonitrile formate, 5% acetonitrile acetate, chloroform, ethyl acetate), 7 extraction times (0 min ~ 5 min ~ 10 min ~ 15 min ~ 20 min ~ 25 min ~ 30 min) and five concentration temperature (30 鈩，

本文編號：2360844