Marine Fisheries Research Institute of Shandong Province, Yantai 264006, PR China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2012 Jun 15;899:14-20. doi: 10.1016/j.jchromb.2012.04.028. Epub 2012 May 4.
A rapid and simple method for the determination of colistin A and B in fishery products by reversed phase ultra performance liquid chromatography with positive electrospray ionization tandem spectrometry (UPLC-ESI-MS/MS) method was described. The samples were extracted with 1.0 mol/L of hydrochloric acid in methanol-water and then purified on the PLS solid phase extraction columns. Then the eluate was evaporated to less than 1 mL under a gentle stream of nitrogen at 40 °C and formic acid-acetonitrile-water (0.2/10/90, v/v/v) was added to adjust volume to 1 mL final volume. An aliquot (10 μL) was injected onto the LC column for analysis with the mobile phase of 0.2% formic acid in acetonitrile and 0.2% formic acid in water at 0.20 mL min⁻¹. Multiple reaction monitoring was performed using precursor-product ion combinations. Calibration curves were linear from 200 ng/mL to 2000 ng/mL for colistin A and B. Mean recoveries were between 72.9% and 82.9%. The LOD was 10.0 μg/kg and LOQ was 40.0 μg/kg. The intra-day assay precision values for QC samples were between 2.17% and 9.00%, and inter-day values were between 2.80% and 6.97%. The method has merits of simplicity, sensitivity and rapidity, and it can be used for the determination of colistin A and B in fishery products.
建立了一种利用反相超高效液相色谱-电喷雾串联质谱法（UPLC-ESI-MS/MS）快速测定水产品中多黏菌素 A 和 B 的方法。样品用甲醇-水（1.0mol/L 盐酸）提取，经 PLS 固相萃取柱净化，氮气流下 40°C 浓缩至近干，用甲酸-乙腈-水（0.2/10/90，v/v/v）定容至 1mL。取 10μL 进样，以 0.2%甲酸乙腈溶液和 0.2%甲酸水溶液为流动相，流速为 0.20mL/min，采用多反应监测模式进行检测。多黏菌素 A 和 B 在 200ng/mL 至 2000ng/mL 范围内线性关系良好，平均回收率为 72.9%82.9%，方法的检出限为 10.0μg/kg，定量限为 40.0μg/kg。在不同添加浓度下，QC 样品日内和日间精密度的相对标准偏差（RSD）均在 2.17%9.00%之间。该方法简便、快速、灵敏，可用于水产品中多黏菌素 A 和 B 的检测。
