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当前位置: 首页 > 文章 > 固相萃取-高效液相色谱-串联质谱法测定牛乳和猪肉中5种青霉素类抗生素 食品科学 2014,35 (24) 308-311
Position: Home > Articles > Determination of 5 Penicillin Residues in Milk and Pork by SPE-HPLC-MS-MS FOOD SCIENCE 2014,35 (24) 308-311

固相萃取-高效液相色谱-串联质谱法测定牛乳和猪肉中5种青霉素类抗生素

作  者：
刘莉萍
单  位：
深圳职业技术学院
关键词：
固相萃取;高效液相色谱-串联质谱;青霉素;牛乳;猪肉
摘  要：
建立一种用固相萃取-高效液相色谱-串联质谱法检测牛乳和猪肉中苄星青霉素G、氨苄西林、苯唑西林、氯唑西林、双氯西林5种青霉素类抗生素方法。样品经乙腈提取,Bond Elut C18固相萃取柱净化,用高效液相色谱-串联质谱检测,外标法定量。结果表明,本方法5种青霉素在2.0~200μg/L范围内呈良好线性关系,线性相关系数大于0.999;牛乳样品添加回收实验,回收率为85.2%~122.7%,相对标准偏差为3.43%~16.8%(n=6);猪肉样品添加回收实验在50μg/kg和100μg/kg添加水平,除氨苄西林外,回收率在94.3%~116.4%,相对标准偏差为1.62%~5.09%(n=6)。方法定量限为1.0~2.0μg/kg。该方法具有简便快捷、准确度高、定量限低的优点,适用于牛乳和猪肉中青霉素类抗生素的测定。
译  名：
Determination of 5 Penicillin Residues in Milk and Pork by SPE-HPLC-MS-MS
作  者：
LIU Li-ping;Shenzhen Polytechnic;
关键词：
solid-phase extraction;;high performance liquid chromatography-tandem mass spectrometry(HPLC-MS-MS);;penicillins;;milk;;pork
摘  要：
A method was established for the determination of 5 penicillin residues in milk and pork by solid-phase extraction and high performance liquid chromatography-tandem mass spectrometry(SPE-HPLC-MS-MS). The samples were extracted with acetonitrile, purified on a Bond Elut C18 column by solid-phase extraction, and finally detected by HPLC-MS-MS and quantified by an external standard method. As a result, the method showed a good linearity with a correlation coefficient higher than 0.999 in the range from 2.0 to 200 μg/L for 5 penicillin compounds. The average recoveries of these five penicillins in milk were in the range of 85.2% to 122.7% with relative standard deviations(RSDs) of 3.43% to 16.8%(n = 6). As for pork samples spiked at 50 and 100 μg/kg, the average recoveries were between 94.3% and 116.4% except for ampicillin with RSDs of 1.62% to 5.09%. The limit of quantification(LOQ) was in the range of 1.0–2.0 μg/kg. In conclusion, the method is convenient, rapid, accurate and sensitive so that it can be applied to determinate penicillin residues in milk and pork.

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