【作者】 雒丽丽；

【导师】 梁琪； 薄海波；

【作者基本信息】 甘肃农业大学 ， 营养与食品卫生学， 2009， 硕士

【摘要】 聚醚类抗生素又称离子载体抗生素,是目前广泛使用的高效、广谱抗球虫药,也可作为畜禽的促生长剂。过量地使用这种抗生素会导致动物产品中残留,甚至会造成畜禽动物的中毒或死亡。本研究以外标法为定量手段,以全脂牛奶、低脂牛奶、鲜牛奶、全脂奶粉、婴儿钙化奶粉、脱脂奶粉为材料,建立了一种专属、灵敏的超高效液相色谱-串接质谱法检测六种聚醚类抗生素残留的分析方法。结果表明:1.二氯甲烷、甲醇和乙酸乙酯作为提取剂时,样品的平均回收率在10.52%～70.13%,而乙腈作为提取剂时,样品的平均回收率均可达到70%以上,确定提取溶剂为乙腈。2.固相萃取法和凝胶渗透色谱法作为净化方法时,样品的平均回收率在15.21%～65.40%,而液液萃取法作为净化方法时,样品的平均回收率均可达到71.20%以上,故选取液液萃取法作为净化方法。3.色谱条件为:色谱柱温度40℃;流速0.25 mL /min;流动相甲醇+0.1%甲酸-5 mmol/L的乙酸铵(90:10,v:v);进样量:5.0μL。质谱条件:毛细管电压2.8 KV;离子源温度110℃;去溶剂气温度380℃;去溶剂气(氮气)流量600 L/hr。4.在此条件下,六种抗生素在0.5μg/Kg～100μg/Kg浓度范围内呈线性,相关系数r>0.99。在空白样品中,添加拉沙洛素、莫能菌素、尼日利亚菌素、盐霉素、甲基盐霉素和马杜拉霉素的回收率分别在75.62%～112.55%、78.25%～112.13%、74.89%～108.10%、78.11%～108.94%、74.60%～114.20%、78.70%～115.64%之间,精密度(RSD)分别为4.97%～12.88%、3.91%～13.76%、5.34%～13.68%、4.40%～13.94%、4.19%～13.42%、3.94%～12.59%之间,最低检测限分别为0.2μg/Kg、0.1μg/Kg、0.1μg/Kg、0.2μg/Kg、0.1μg/Kg、0.3μg/Kg。本实验建立方法可应用于牛奶和奶粉中六种聚醚类抗生素残留的检测。更多还原

【Abstract】 Polyether antibiotics, also known as ionophore antibiotic, was widely used as high- efficiency, broad-spectrum anti-Coccidiostats, can also be used as animal growth-promoting agent. To use this antibiotics excessiveLy will lead to residues in animal food, or even cause animal poisoning or death.In this study, Selected full fat milk, low fat milk, fresh milk, full fat powdered milk, calcification of powdered milk for infant, skimmed fat milk as samples, a sensitive and selective method was developed for determination of six Polyether antibiotics residues in milk and powdered milk. Using external standard method.The results show:First: Dichloromethane, methanol and ethyl acetate as extractions, the average recovery rate of samples between 10.52% and 70.13%, but acetonitrile as the extraction, the average recovery rate of samples was over 70%, so the extraction was acetonitrile. Second: Solid-phase extraction method and gel permeation chromatography as a clean-up method, the average recovery rate of samples between 15.21% and 65.40%, but liquid-liquid extraction as a clean-up method, the average recovery rate of samples was over 71.20%, so liquid-liquid extraction was the clean-up method.Third: Chromatographic conditions: Methanol +Formic acid of 0.1%-Ammonium acetate of 5 mmol/L (90:10,v:v) as its mobile, the flow rate was 0.25 mL/min, column temperature was at 40℃. MS conditions: the capillary cone was 2.8 KV; ion source temperature was 110℃; desolvation temperature was 380℃; desolvation gas flow was 600 L/hr.Fourth: The operating ranges of the chromatographic analysis were determined. Calibration graphs were good linearity over the concentration ranges tested (0.5μg/Kg～100μg/Kg, R>0.99). The average recoveries from spiked milk and powdered milk at the three concentrations of 0.5, 10.0, 20.0μg/Kg ranged from 75.62%～112.55%、78.25%～112.13%、74.89%～108.10%、78.11%～108.94%、74.60%～114.20%、78.70%～115.64% respectively; with relative standard deviation ranged from 4.97%～12.88%、3.91%～13.76%、5.34%～13.68%、4.40%～13.94%、4.19%～13.42%、3.94%～12.59% respectively; and the limits of detection were 0.2μg/Kg、0.1μg/Kg、0.1μg/Kg、0.2μg/Kg、0.1μg/Kg、0.3μg/Kg respectiveLy in milk and powdered milk. Our experiment used liquid chromatography with mass pectrometry was confirmed, it was applied to detect six Polyether antibiotics residual in milk and powdered milk.更多还原