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目的:采用超高效液相色谱法(UPLC)测定呼和浩特市12个自来水水厂的微囊藻毒素-LR。方法:取水样5 L,GF/C过滤,滤液过C18柱,依次用50 ml去离子水,50 ml 20%甲醇淋洗,50 ml 80%甲醇洗脱,氮气吹干,残渣溶于1 ml甲醇,过0.45 um滤膜进样。采用C18色谱柱,流动相为乙腈+水+三氟乙酸(38+62+0.01),流速0.2 ml/min,PDA检测器检测。结果:微囊藻毒素-LR在0.3μg/ml~2.0μg/ml范围内线性良好(r=0.9998),且峰形好,回收率为70%~85%,精密度RSD为1.0%~5.0%,检出限为0.05μg/ml。结论:本法定性准确、灵敏度高、回收率和重现性好,操作快速。
OBJECTIVE: To determine microcystin-LR of 12 waterworks in Hohhot by using ultra performance liquid chromatography (UPLC). Methods: Take 5 L of water and filter with GF / C. The filtrate was passed through C18 column, rinsed with 50 ml of deionized water, 50 ml of 20% methanol and 50 ml of 80% methanol. The residue was dissolved in 1 ml methanol, over 0.45 um filter injection. Using C18 column, the mobile phase was acetonitrile + water + trifluoroacetic acid (38 + 62 + 0.01), the flow rate was 0.2 ml / min, detected by PDA detector. Results: The microcystin-LR showed a good linearity (r = 0.9998) in the range of 0.3μg / ml ~ 2.0μg / ml and the peak shape was good with the recovery of 70% ~ 85% and the precision RSD of 1.0% ~ 5.0 %, The detection limit of 0.05μg / ml. Conclusion: This method is accurate and accurate, high sensitivity, good recovery and reproducibility, and fast operation.