Meinertz J R, Stehly G R, Gingerich W H
U.S. Geological Survey, Biological Resources Division, Upper Mississippi Science Center, La Crosse, WI 54602-0818, USA.
J AOAC Int. 1998 Jul-Aug;81(4):702-8.
The approved use of oxytetracycline (OTC) in U.S. aquaculture is limited to specific diseases in salmonids and channel catfish. OTC may also be effective in controlling diseases in other fish species important to public aquaculture, but before approved use of OTC can be augmented, an analytical method for determining OTC in fillet tissue from multiple species of fish will be required to support residue depletion studies. The objective of this study was to develop and validate a liquid chromatographic (LC) method that is accurate, precise, and sensitive for OTC in edible fillets from multiple species of fish. Homogenized fillet tissues from walleye, Atlantic salmon, striped bass, white sturgeon, rainbow trout, and channel catfish were fortified with OTC at nominal concentrations of 10, 20, 100, 1000, and 5000 ng/g. In tissues fortified with OTC at 100, 1000, and 5000 ng/g, mean recoveries ranged from 83 to 90%, and relative standard deviations (RSDs) ranged from 0.9 to 5.8%. In all other tissues, mean recoveries ranged from 59 to 98%, and RSDs ranged from 3.3 to 20%. Method quantitation limits ranged from 6 to 22 ng/g for the 6 species. The LC parameters produced easily integratable OTC peaks without coelution of endogenous compounds. The method is accurate, precise, and sensitive for OTC in fillet tissue from 6 species of fish from 5 phylogenetically diverse groups.
在美国水产养殖中，土霉素（OTC）的批准用途仅限于鲑科鱼类和斑点叉尾鮰的特定疾病。OTC可能对控制其他对公共水产养殖重要的鱼类疾病也有效，但在扩大OTC的批准用途之前，需要一种用于测定多种鱼类鱼片组织中土霉素的分析方法，以支持残留量消减研究。本研究的目的是开发并验证一种液相色谱（LC）方法，该方法对多种鱼类可食用鱼片中的土霉素准确、精密且灵敏。用土霉素以10、20、100、1000和5000 ng/g的标称浓度强化来自大眼狮鲈、大西洋鲑、条纹鲈、白鲟、虹鳟和斑点叉尾鮰的匀浆鱼片组织。在以100、1000和5000 ng/g的土霉素强化的组织中，平均回收率为83%至90%，相对标准偏差（RSD）为0.9%至5.8%。在所有其他组织中，平均回收率为59%至98%，RSD为3.3%至20%。6种鱼类的方法定量限为6至22 ng/g。LC参数产生易于积分的土霉素峰，且无内源性化合物共洗脱。该方法对来自5个系统发育不同类群的6种鱼类的鱼片组织中的土霉素准确、精密且灵敏。
