固相萃取-高效液相色谱法测定α-乙酰乳酸脱羧酶中四环素残留量  被引量:3

Decarboxyl Enzyme by High Performance Liquid Chromatography

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作  者:李浩 

机构地区:[1]广西壮族自治区食品药品检验所,广西南宁530021

出  处:《食品与发酵科技》2015年第1期91-95,共5页Food and Fermentation Science & Technology

摘  要:建立高效液相色谱法测定α-乙酰乳酸脱羧酶中四环素残留量。样品经EDTA-Mcllvaine缓冲液提取,通过Oasis HLB固相萃取柱净化后,V(甲醇)∶V(乙酸乙酯)=1∶9溶液洗脱,氮气流下浓缩定容,采用资生堂ACR(4.6mm×150mm×5μm)色谱柱,以草酸(0.01mol/L)-乙腈-甲醇(82∶12∶6)为流动相,流速为1m L/min进行测定。四环素检测限(LOD)为0.04043mg/kg,进样量在0.0904-15.07mg/kg范围内线性关系良好,相关系数r=0.9998,样品加标回收率为77.5%,RSD为2.6%。本实验建立的方法简便灵敏,结果准确可靠,重现性好,适用于食品中四环素类药物残留量的测定。To establish a HPLC method for the determination of teracycliny residual in α-aceryl lactic decarboxyl enzyme. Samples were extracted by EDTA-Mcllvaine buffer and cleaned up by Oasis HLB column.The column was washed by methanol-ethyl acetate.The elution was dried under nitrogen, dissolved in mobile phase. The mycotoxins were separated on a ACR(4.6mm×150mm×5μm) and using mobile phase of oxalic acid-acetonitrile-methanol, the flow rate was 1ml per minute. The limits of detection(LOD) of tetracycline was 0.04043mg/kg, the results showed that the sample was in good linear at the range of 0.0904-15.07mg/kg(r=0.9998). The average recovery rate was77.5%, and the RSD was 2.6%. The method is simple, sensitive, accurate and good reproducibility, proved to be applicable in determination of tetracycline residual in food.

关 键 词:Α-乙酰乳酸脱羧酶 高效液相色谱法 四环素残留 

分 类 号:TS207.3[轻工技术与工程—食品科学]

 

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