动物源性食品中磺胺类药物残留量检测方法的研究
发布时间：2018-11-27 12:51
【摘要】：磺胺类药物(Sulfonamides,SAs)是指拥有对氨基苯磺酰胺结构的一类药物的总称[1]。该类药物因抗菌效果好、价格低廉等特点,使其在养殖领域得到广泛应用。但因一些不规范添加及使用,磺胺类药物会在动物体内残留,食用这些超标的食物后,会引起人体的过敏反应、毒性反应,产生抗药性、引起“三致”(致畸、致癌和致突变)作用等。因此,从食品安全角度出发,对动物源性食品中磺胺类药物残留量检测问题一直较为关注。动物源性食品中磺胺类药物残留量的检测方法一直在不断更新和提高中,液质联用技术因为其选择性、灵敏度、分析效能等方面的优势,是目前最常用的检测方法,但其在实际检测应用中,常使用到三氯甲烷、丙酮等有机溶剂,如果操作不当,将会对实验人员的身体操成伤害;而且大量使用有机溶剂也会大大增加检测成本,对环境会有一定的破坏。本研究运用液质联用改进技术,旨在减少有机溶剂的使用,减少实验成本,提高检测效率。重点研究并确定了五种提取溶剂(5%甲酸乙腈、5%乙酸乙腈、乙腈、三氯甲烷、乙酸乙酯),7种提取时间(0min、5min、10min、15min、20min、25min、30min),5个浓缩温度(30℃、40℃、50℃、60℃、70℃),4种色谱柱(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)对实验结果的影响。本试验确定了用于16种动物源性食品磺胺残留的检测方法,检测结果显示:16种磺胺在1~50μg/L范围内的线性相关系数(R2)为0.9965~0.9994,16种磺胺的加标回收率为85.82~109.51%,相对偏差为2.30~11.25%,检出限为0.003~0.022μg/kg,定量限为0.2~1.1μg/kg。具体操作和检测过程如下:样品采用5%乙酸乙腈作为提取溶剂,提取20min,采用Bond ElutQuechers EM提取盐、EMR-Lipidstp和EMR-polish管简便、无毒的方法,对样品进行净化。在50℃的条件下用氮吹浓缩,采用C_(18)-MGⅢ(pH 2-10)3μm 2.0mmI.D.×150mm柱作为本试验的色谱柱。通过与国标法(GB/T 20759-2006)检测结果进行对比,相对偏差在4.28-9.76%之间。本测准方法准确率高,且有机溶剂用量较少,成本低,效率高,适用于动物源性食品中磺胺类药物残留的检测。
[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，
本文编号：2360844
[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，
本文编号：2360844
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