Determination of tetracycline antibiotics in beef and pork tissues using ion-paired liquid chromatography.
Determination of tetracycline antibiotics in beef and pork tissues using ion-paired liquid chromatography.
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DOI：
10.1021/jf990649r
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发表时间：
2000-05
影响因子：
6.1
通讯作者：
W. A. Moats
中科院分区：
文献类型：
--
作者：
W. A. Moats
本文提出了一种测定组织中四环素类抗生素的简化方法，提高了样品提取物中四环素类抗生素的稳定性，并省去了繁琐的净化程序。将组织在水中均质化。向4 mL匀浆中加入乙腈（16 mL），然后加入1 mL 0.1 M H（3）PO（4），过滤澄清上清液。将滤液与己烷和二氯甲烷混合，收集所得水层，蒸发至1-2 mL，并过滤至自动进样器小瓶中。离子对液相色谱法用于分离样品提取物中的干扰四环素，消除了进一步净化的需要。使用Phenomonex Prodigy ODS（3）柱进行等度分析，柱中移动的流动相为4 mM草酸、4 mM草酸钠、10 mM癸烷磺酸钠-乙腈（土霉素和四环素为70 + 30;金霉素为66 + 34）。回收率通常在90-100%范围内，定量限为0。05-0.1 ppm。用牛肉和猪肉、肝脏和肾脏对该程序进行了评价。
A simplified procedure was developed for determination of tetracycline antibiotics in tissues which improved stability of these compounds in sample extracts and eliminated the need for troublesome cleanup procedures. Tissues were homogenized in water. Acetonitrile (16 mL) and then 1 mL of 0.1 M H(3)PO(4) were added to 4 mL of homogenate and the clear supernatant was filtered. The filtrate was mixed with hexane and dichloromethane and the resulting water layer was collected, evaporated to 1-2 mL, and filtered into autosampler vials. Ion-pairing liquid chromatography was used to separate tetracyclines from interferences in sample extracts, eliminating the need for further cleanup. Analysis was isocratic using a Phenomonex Prodigy ODS(3) column with a mobile phase of 4 mM oxalic acid, 4 mM sodium oxalate, 10 mM sodium decanesulfonate-acetonitrile (70 + 30 for oxytetracycline and tetracycline; 66 + 34 for chlortetracycline). Recoveries were generally in the 90-100% range with limits of quantitation of 0. 05-0.1 ppm. The procedure was evaluated with beef and pork muscle, liver, and kidney.