Kawata S, Sato K, Nishikawa Y, Iwama K
Yokohama City Meat Inspection Office, Japan.
J AOAC Int. 1996 Nov-Dec;79(6):1463-5.
A simple and rapid method was developed for determination of oxytetracycline (OTC) in swine muscle and kidney by liquid chromatography (LC). The method involved homogenization of sample in acetonitrile-1M imidazole buffer containing 10 mM disodium ethylenediaminetetraacetic acid (Na2.EDTA) and 50 mM magnesium acetate (15 + 85) with added hexane, centrifugation, removal of the hexane phase, and ultrafiltration of the supernatant. L-column ODS (150 x 4.6 mm) with a mobile phase of acetonitrile-1M imidazole buffer containing 50 mM magnesium acetate and 10 mM Na2.EDTA (10 + 90) was used for the LC separation. A fluorescence detector was used at an excitation wavelength of 380 nm and an emission wavelength of 520 nm. The calibration graph was linear from 1.25 to 200 ng OTC. Recoveries of OTC from swine tissue fortified at levels of 0.05-1.0 microgram/g ranged from 58.0 to 67.3%. The quantitation and detection limits were 0.05 and 0.04 microgram/g, respectively.
开发了一种简单快速的液相色谱法（LC）测定猪肌肉和肾脏中土霉素（OTC）的方法。该方法包括将样品在含有10 mM乙二胺四乙酸二钠（Na2.EDTA）和50 mM乙酸镁的乙腈-1M咪唑缓冲液（15 + 85）中匀浆，加入己烷，离心，去除己烷相，然后对上清液进行超滤。使用L-column ODS（150 x 4.6 mm），流动相为含有50 mM乙酸镁和10 mM Na2.EDTA的乙腈-1M咪唑缓冲液（10 + 90）进行LC分离。使用荧光检测器，激发波长为380 nm，发射波长为520 nm。校准曲线在1.25至200 ng OTC范围内呈线性。在0.05 - 1.0微克/克水平加标的猪组织中，OTC的回收率为58.0%至67.3%。定量限和检测限分别为0.05和0.04微克/克。
