Gu Congying, Lin Li, Fang Nenghu, Jia Jinping
College of Environmental Science and Engineering, Shanghai Jiao Tong University, Shanghai 200240, China.
Se Pu. 2007 Mar;25(2):174-8.
Polymethacrylate-based monolithic column was prepared in 150 microm i. d. capillary column in situ using butylmethacrylate and ethylene dimethacrylate. The application of methacrylate monolithic column in capillary high performance liquid chromatography ( micro-HPLC) for separation of microcystins (MCs) with ultraviolet (UV) detection has been studied. The properties of the monolithic column could be easily tailored by altering the preparation conditions. For the good reproducibility in preparation of monolithic column, this method could be used for the analysis of samples in practical. The effects of composition of mobile phase, pH value, concentration of the buffer, and the flow rate of the mobile phase on the separation of microcystins were investigated. The optimum separation for microcystins, MC-LR, MC-YR, and MC-RR, was achieved with a gradient elution of mobile phase A (0. 01 mol/L phosphate buffer, pH 2. 5 ) and mobile phosphate B (acetonitrile). The standard microcystins could be baseline-separated within 9 min. The limits of detection (LODs) (S/N = 3) for three standard microcystins were in the range of 0. 80 - 1. 03 mg/L. The intra-day and inter-day precisions of the method were obtained with the values of relative standard deviation less than 1. 0% and 2. 0%, respectively. This method was successfully used to analyze bloom samples and laboratory-cultured samples of cyanobacteria after performing solid phase extraction (SPE) using C18 cartridges for preconcentration. The whole procedure provided low LODs for MCs, e. g. the LOD for MC-LR was found to be 420 ng/L. This family of microcystin is analyzed by VL-HPLC using methacrylate monolithic column for the first time. It is shown that this method is promising in the routine analysis of microcystins in water samples in practical.
采用甲基丙烯酸丁酯和二甲基丙烯酸乙烯酯在150微米内径的毛细管柱中原位制备了基于聚甲基丙烯酸酯的整体柱。研究了甲基丙烯酸酯整体柱在毛细管高效液相色谱（微HPLC）中用于微囊藻毒素（MCs）分离并结合紫外（UV）检测的应用。通过改变制备条件，可以轻松调整整体柱的性能。由于整体柱制备具有良好的重现性，该方法可用于实际样品的分析。研究了流动相组成、pH值、缓冲液浓度和流动相流速对微囊藻毒素分离的影响。采用流动相A（0.01 mol/L磷酸盐缓冲液，pH 2.5）和流动相B（乙腈）梯度洗脱，实现了微囊藻毒素MC-LR、MC-YR和MC-RR的最佳分离。标准微囊藻毒素可在9分钟内实现基线分离。三种标准微囊藻毒素的检测限（S/N = 3）在0.80 - 1.03 mg/L范围内。该方法的日内和日间精密度分别为相对标准偏差小于1.0%和2.0%。该方法在使用C18柱进行固相萃取（SPE）预浓缩后，成功用于分析蓝藻水华样品和实验室培养样品。整个过程对微囊藻毒素提供了低检测限，例如MC-LR的检测限为420 ng/L。首次采用甲基丙烯酸酯整体柱通过VL-HPLC分析了该类微囊藻毒素。结果表明，该方法在实际水样中微囊藻毒素的常规分析中具有应用前景。
