建立了直接进样-高效液相色谱-串联四极杆质谱分析环境水样中微囊藻毒素-LR的分析方法。方法使用C18反相柱为分离柱，柱温40℃，流速0.7 mL/min，乙腈和甲酸水溶液(0.1％)作流动相，采用梯度洗脱，保留时间4.13 min。串联质谱采用多反应监测模式，使用ESI (﹢)源电离水样。在上述条件下，水样过粒径为0.45μm的滤头后可直接进样，进样体积25μL时检出限可达0.04μg/L，在0.10~200μg/L范围内线性良好( R＝0.9998)；样品加标回收率为96.6％~106％，相对标准偏差为1.3％~5.6％。同时方法应用到实际环境水样分析中也具有令人满意的结果。该方法灵敏度高，快速简单，适用于环境水样中MC-LR的分析。%A new method was developed for determine MC-LR in water sample by high performance liquid chromatography tandem mass spectrometry ( HPLC-MS/MS ) . Chromatographic separation was performed on C18 reversed phase column, column temperature was 40 ℃, flow rate was 0. 7 mL/min, used Acetonitrile and Formic Acid as mobile phase, gradient elution, retention time was 4. 13 min. MC-LR in water was cleaned by 0. 45 μm Millipore filter, then detected by HPLC-MS/MS. Identification was achieved by electro spray ionization ( ESI) in multiple reaction monitoring mode. The detection limit of the method was 0. 04 μg/L. The calibration curve showed good linearity over the tested range from 0. 10 to 200μg/L with correlation of 0. 999 8. The recoveries ranged from 96. 6% to 106%,and RSDs ranged from 1. 3% to 5. 6%. The proposed method was successfully applied to determine MC-LR in actual water sample. This method was sensitive, fast, simple and therefore can be used for determination of MC-LR in water sample.
展开▼
