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建立了超高效液相色谱-三重四极杆质谱快速检测水中12种微囊藻毒素(MCs)和1种节球藻毒素(NOD)的分析方法。水样经甲醇等体积稀释,聚醚砜(PES)滤膜过滤,滤液直接进样分析,以0.1%(v/v)甲酸乙腈溶液和0.2%(v/v)甲酸水溶液作为流动相进行梯度洗脱,采用ACQUITY UPLC BEH 300 C18柱(100 mm×2.1 mm,1.7μm)进行分离,在电喷雾正离子模式下以MRM方式进行检测,标准溶液外标法定量。方法的检出限为0.03~0.1μg/L,定量限为0.1~0.3μg/L。对自来水和河水样品进行加标回收试验,目标物的平均加标回收率为79.5%~123%,相对标准偏差为1.0%~20%(n=6)。该法简单、灵敏、准确,适用于水中12种微囊藻毒素和1种节球藻毒素的快速测定。 相似文献
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建立了同时检测淡水鱼中柱孢藻毒素、节球藻毒素、微囊藻毒素-RR、微囊藻毒素-YR及微囊藻毒素-LR的分散固相萃取-液相色谱-串联质谱方法。样品粉碎后,用乙腈-水-甲酸(89 ∶ 10 ∶ 1,v/v/v)提取目标物,C18分散固相萃取柱净化,Agilent ZORBAX Eclipse XDB C18色谱柱分离,乙腈和水梯度洗脱,在多反应监测(MRM)模式下进行定性分析,基质匹配标准曲线外标法定量。考察了提取溶剂及吸附剂种类对提取效率和净化效果的影响,并优化了液相色谱-串联质谱条件。该法在各自范围内具有良好线性关系,相关系数(R2)≥0.9954;检出限为5~10 μg/kg,定量限为15~40 μg/kg;样品的加标回收率为62.3%~101.2%。该方法前处理方法简单快速,灵敏高效,适用于淡水鱼中柱孢藻毒素、节球藻毒素和微囊藻毒素的有效检测。 相似文献
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A LC-MS/MS method with enhanced sensitivity and specificity was established for monitoring microcystin-LR (MC-LR) in drinking water supplies in southern Taiwan. The enhanced sensitivity was achieved by the selection of a doubly charged MC-LR as the precursor ion to result in an multiple reaction monitoring (MRM) pair ions of m/z 498.6 --> 135.0. Using this ion pair, a record low detection limit of 2 pg was achieved on column, found in the available literature. A sample preparation method involving C8 solid-phase extraction gave satisfactory recoveries of the analyte. Nodularin, with structural similarity to MC-LR, was used as an internal standard to minimize matrix effects of water samples collected from six different water reservoirs in southern Taiwan, where MC-LR was detected at sub-ppb levels in all the reservoirs. The best precision and accuracy of this method were found with samples prepared to contain MC-LR at 0.1 and 1 microg l(-1). This new method requires considerably smaller water sample volumes because of enhanced quantification sensitivity and hence reduces the time needed for analysis. It should serve as a useful example for method development for monitoring other members of the microcystin family in drinking water supplies. 相似文献
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