College of Bioscience and Biotechnology, Chubu University, Kasugai-shi, Aichi, Japan.
J Sep Sci. 2011 Jul;34(13):1525-30. doi: 10.1002/jssc.201100112. Epub 2011 May 13.
A simple, selective and rapid analytical method for determination of trimethoprim (TMP) in honey samples was developed and validated. This method is based on a SPE technique followed by HPLC with photodiode array detection. After dilution and filtration, aliquots of 500 μL honey samples were directly injected to an on-line SPE HPLC system. TMP was extracted on an RP SPE column, and separated on a hydrophilic interaction chromatography column during HPLC analysis. At the first detection step, the noise level of the photodiode array data was reduced with two-dimensional equalizer filtering, and then the smoothed data were subjected to derivative spectrum chromatography. On the second-derivative chromatogram at 254 nm, the limit of detection and the limit of quantification of TMP in a honey sample were 5 and 10 ng/g, respectively. The proposed method showed high accuracy (60-103%) with adequate sensitivity for TMP monitoring in honey samples.
建立并验证了一种用于蜂蜜样品中甲氧苄啶（TMP）测定的简单、选择性和快速的分析方法。该方法基于 SPE 技术，结合 HPLC 与光电二极管阵列检测。样品经稀释和过滤后，直接取 500μL 等分试样注入在线 SPE-HPLC 系统。TMP 在反相 SPE 柱上被提取，在 HPLC 分析中于亲水相互作用色谱柱上被分离。在第一个检测步骤中，使用二维均衡滤波器降低光电二极管阵列数据的噪声水平，然后对平滑数据进行导数谱色谱分析。在 254nm 处的二阶导数色谱图中，蜂蜜样品中 TMP 的检测限和定量限分别为 5 和 10ng/g。该方法具有较高的准确性（60-103%），对蜂蜜样品中 TMP 的监测具有足够的灵敏度。
