液质联用法快速、同时测定水中的呋喃丹、莠去津、西维因和微囊藻毒素LR

Rapid and simultaneous determination of carbofuran,atrazine,carbaryl and microcystis LR in water by LC-MS / MS method

目的为提高实验室水质检测效率,研究建立快速、同时测定水中呋喃丹、莠去津、西维因和微囊藻毒素LR的HLB固相萃取柱富集净化-液相色谱质谱联用分析的方法。方法水样品经0.45μm滤膜过滤后,通过Waters HLB固相萃取柱富集和净化,以Waters ACQUITY UPLCBEH C18(2.1 mm×50 mm,1.7μm)色谱柱为分离柱,以乙腈-0.1%甲酸为流动相,梯度洗脱,质谱仪以MRM模式检测,分析时间仅为2.5 min。结果呋喃丹、莠去津和西维因的线性范围为4 ng/L^400 ng/L,微囊藻毒素LR的线性范围为20 ng/L^2 000 ng/L。呋喃丹、莠去津、西维因和微囊藻毒素LR的平均加样回收率分别为88.82%、86.42%、82.92%和98.43%,相对标准偏差为1.49%~7.78%。结论本方法能有效提高实验室水质检测效率,且方法的定量下限远低于国家标准规定的最高限量,具有较好的检测灵敏度。

Objective To improve the detection efficiency, a method of rapid and simultaneous determination of carbofuran, at- razine, carbaryl and microcystis LR in water by LC - MS/MS method coupled with HLB solid phase extraction was established in this study. Methods After filtrated by 0.45μm microporous membrane, water sample was concentrated and purified in Waters HLB SPE column. Four toxins in the water sample were separated on Waters ACQUITY UPLC BEH C18（2.1 mm ×50 mm, 1.7 μm） chromatographic column with mobile phase of acetonitrile and 0.1% formic acid solution, and detected by mass spec- trometer in multi - reaction monitoring （MRM） mode. The total procedure took about 2.5 minutes. Results The linear range of carbofuran, atrazine or carbaryl was 4 ng/L - 400 ng/L, and the range of microcystis LR was 20 ng/L - 2 000 ng/L. Extrac- tion recoveries of carbofuran, atrazine, carbaryl and microcystis LR were 88.82 %, 86.42 %, 82.92 %, 98.43 %, respectively, with RSDs in the range of 1.49% -7.78%. Conclusion This established method could quickly quantify carbofuran, atrazine, carbaryl and microcystis LR in water, with a lower LLOQ compared with government standard.