高效液相色谱-串联质谱法测定牛奶中6种青霉素类药物的残留量  被引量:24

Determination of six penicillins residues in milk by LC-MS/MS

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作  者:秦峰[1,2] 郑文捷[1] 陈桂良[2] 仇士林[2] 

机构地区:[1]上海交通大学,上海200032 [2]上海市食品药品检验所,上海201203

出  处:《中国抗生素杂志》2009年第6期348-351,共4页Chinese Journal of Antibiotics

摘  要:目的建立一种高效液相串联质谱法,快速测定牛奶中6种青霉素类抗生素的残留量。方法样品经乙腈沉淀蛋白,正己烷脱脂,氮吹浓缩,经高效液相色谱C18柱分离,选用含0.1%甲酸的水溶液和0.1%甲酸的乙腈溶液作流动相,在22min内梯度洗脱将6种青霉素类抗生素得以分离。结果方法检出限为青霉素G0.5ng/ml、青霉素V1.0ng/ml、苯唑西林1.0ng/ml、氯唑西林2.0ng/ml、阿莫西林2.0ng/ml以及双氯西林1.0ng/ml,在0.5~20ng/ml线性范围内,相关系数r均大于0.990,平均回收率均大于80%。结论该方法前处理过程快速,结果准确可靠,灵敏度高。Objective To establish a method for the detection of 6 penicillin residues in milk by HPLC-MS/ MS. Method The sample was extracted and degreaseds by acetonitrile and n-hexane ,the extract was concentrated by nitrogen. The chromatography was performed by reversed phase HPLC in a C18 column. The mobile phase was acetonitrile (0.1% formic acid ) and water (0.1% formic acid). Six kinds of penicillin antibiotics were separated by gradient elution in 22 minutes. Results The limit of quantization of six penicillins were 0.5 - 2.0 ng/ml , correlation coefficient were above 0. 990 within the linear range of 0.5 - 20 ng/ml. The average recovery was above 80%. Conclusion The pre-treatment process of the method is rapid, the results are reliable and high sensitivity.

关 键 词:牛奶 青霉素残留 液相色谱-串联质谱 

分 类 号:R978.1[医药卫生—药品]

 

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