采用高效液相色谱法和二极管阵列检测法测定液体饲料预混剂中的磺胺二甲嘧啶和甲氧苄啶，并分析分析结果的不确定度。

Determination of sulfamethazine and trimethoprim in liquid feed premixes by HPLC and diode array detection, with an analysis of the uncertainty of the analytical results.

作者信息

Cancho Grande B, García Falcón M S, Rodríguez Comesaña M, Simal Gándara J

机构信息

Nutrition and Bromatology Group, Analytical and Food Chemistry Department, Faculty of Food Science and Technology, University of Vigo, Ourense Campus, 32004 Ourense, Spain.

出版信息

J Agric Food Chem. 2001 Jul;49(7):3145-50. doi: 10.1021/jf010071x.

DOI:10.1021/jf010071x

PMID:11453744

Abstract

Sulfamethazine (SMZ) and trimethoprim (TMP) are antibacterials used in veterinary practice. This paper describes a method for their determination in veterinary liquid feed premixes that is based on liquid chromatography with diode array detection. Gradient elution with methanol and ammonium acetate achieved excellent separation of the two analytes within 15 min without any interference from the matrix. Absorbance of the column effluent was monitored at 264 nm for SMZ and at 230 nm for TMP. Detailed analyses of the uncertainties of determinations afford estimated expanded uncertainties of, respectively, 0.2 and 0.1 w/v % for typical SMZ and TMP concentrations of 10.7 and 2.1 w/v %, respectively. At the lower end of the calibrated range of the method, the dominant source of uncertainty is the preparation of standards and the construction of the calibration line.

摘要

磺胺二甲嘧啶（SMZ）和甲氧苄啶（TMP）是兽医临床上使用的抗菌药物。本文描述了一种基于二极管阵列检测液相色谱法测定兽用液体饲料预混剂中这两种药物的方法。用甲醇和醋酸铵进行梯度洗脱，在15分钟内实现了两种分析物的良好分离，且不受基质干扰。在264nm处监测磺胺二甲嘧啶的柱流出物吸光度，在230nm处监测甲氧苄啶的柱流出物吸光度。对测定不确定度的详细分析表明，对于典型浓度分别为10.7w/v%和2.1w/v%的磺胺二甲嘧啶和甲氧苄啶，估计的扩展不确定度分别为0.2和0.1w/v%。在该方法校准范围的下限，不确定度的主要来源是标准品的制备和校准曲线的构建。