牛奶中青霉素残留量检测的方法学探索①(1)
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2010年8月1日
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【摘要】目的 牛奶中抗生素残留问题是目前我国奶制品行业存在的一个非常严重的社会问题和公认的食品安全隐患,同时奶制品又是婴幼儿主要的营养来源,为测定青霉素在牛奶中的残留情况及各种烹调加工方法对它的影响,我们拟初步建立反高效液相色谱法对牛奶中青霉素残留量进行测定的方法。方法 以C18色谱柱、磷酸二氢钾—乙腈流动相、225nm 检测波长、1mL/min流速、20℃柱温、10μL进样量等色谱条件,采用外标法对添加在牛奶中的青霉素进行定量,得出在样品前处理方法条件下测定的线性范围、方法最低检测限、回收率、精密度及标准溶液的稳定性。 结果 青霉素在2--11μg/mL线性范围内有良好的线性关系(r=0.9945),方法最低检测限为8ng/mL。在低(3μg/mL)、中(7μg/mL)、高(9μg/mL)3个质控浓度下,青霉素的回收率分别为115.52%、105.52%、95.35%。精密度分别为 5.8%、8.6%、7.8% ,青霉素标准溶液在4℃ 条件下的稳定性比 20℃ 条件下的稳定性好。结论 初步建立了反高效液相色谱法测定牛奶中青霉素残留量的方法,在目前研究的实验条件下方法达到可接受的精密度、回收率要求。
【关键词】青霉素牛奶高效液相色谱法残留
【中图分类号】S859.84【文献标识码】A 【文章编号】1004-7484(2010)08-0-03
The Exploration of the Determination of the Penicillin Residues in Milk
【Objective】At present, the issue of antibiotic residues in milk is a very serious social problem and recognized food safety problems in dairy industry. Dairy products are the main source of infants’ nutrition. In order to determinate penicillin residues in milk and the impact of a variety of cooking methods on it in the future, we intend to initially establish RP-HPLC of testing penicillin residues in milk.Methods:The outer quantitative analysis method was adopted to quantify penicillin content in the milk, by such chromato- graphic conditions as A C18 column,potassium dihydrogen phosphate - acetonitrile mobile phase, 225nm detection wavelength, flow rate 1mL/min, 20 ℃ column temperature, and 10μL injection volume. The linear range, lowest detectable limit, recovery rate, precision and stability of standard solution of the sample pre- treatment method were obtained. Results: Penicillin in the linear range of 2--11μg/ml is a good linear relationship (r = 0.9945), the lowest detectable limit of method is 8ng/ml. Under low (3μg/ml), mid(7μg/ml) and high (9μg/ml) three quality control concentration, the recovery rate of penicillin are 115.52%, 105.52% and 95.35%, the precision are 5.8%, 8.6% and 7.8%. Stability of penicillin standard solution at 4 ℃ is better than that under the conditions of 20 ℃.Conclusion: The method of RP-HPLC for detecting penicillin content in milk is initially established ......
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