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超高效液相色谱-串联质谱法(UPLC-MS/MS)由于其快速、简便的特点,目前广泛应用于水中微囊藻毒素的测定。由于蓝藻水华样品基质比较复杂,UPLC-MS/MS在复杂基质的分析过程中容易发生基质效应问题,严重影响其定量分析结果的准确性。通过稀释样品、优化梯度洗脱程序、减少进样量等方法有效地降低或消除了基质干扰及基质效应问题。7种目标物在各自线性范围内线性关系良好,相关系数(r2)≥0.99;检出限和定量限分别为0.064~0.103μg/L和0.213~0.343μg/L。通过稀释样品、减少进样量等措施,成功测定了水华爆发时实际样品中的微囊藻毒素,并有效降低了基质效应的干扰。该法为微囊藻毒素的准确测定提供一定的参考,对保障饮用水源地的安全具有十分重要的意义。
Ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS / MS) is widely used in the determination of microcystin in water due to its fast and easy performance. Due to the complexity of cyanobacteria bloom samples, UPLC-MS / MS is susceptible to matrix effects in the analysis of complex matrices and seriously affects the accuracy of quantitative analysis. By diluting the sample, optimizing the gradient elution procedure, reducing the injection volume and other methods to effectively reduce or eliminate the matrix interference and matrix effects. The linearity of the 7 kinds of targets in each linear range was good with the correlation coefficient (r2) ≥0.99. The detection limits and the limits of quantification were 0.064 ~ 0.103μg / L and 0.213 ~ 0.343μg / L, respectively. By diluting the sample and reducing the injection volume, the microcystin in the actual sample was successfully measured and the interference of matrix effect was effectively reduced. The method provides a certain reference for the accurate determination of microcystins and is of great significance for ensuring the safety of drinking water sources.