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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 UPLCBEH 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 efficiency of laboratory water quality testing, a fast and simultaneous determination of carbofuran, atrazine, cisplatin and microcystin LR in water by HLB solid-phase extraction (SPE) column chromatography-mass spectrometry method. Methods The water sample was filtered through 0.45μm membrane and then was separated and purified by Waters HLB SPE. The column was separated on a Waters ACQUITY UPLC BEH C18 (2.1 mm × 50 mm, 1.7μm) column with acetonitrile-0.1 % Formic acid as mobile phase, gradient elution, mass spectrometer MRM mode detection, analysis time is only 2.5 min. Results The linear range of carbofuran, atrazine and cisplatin was 4 ng / L ~ 400 ng / L, and the linear range of microcystin LR was 20 ng / L ~ 2 000 ng / L. The average recoveries of carbofuran, atrazine, cisplatin and microcystin LR were 88.82%, 86.42%, 82.92% and 98.43%, respectively, and the relative standard deviations were 1.49% ~ 7.78%. Conclusion This method can effectively improve the efficiency of laboratory water quality testing, and the quantitative lower limit of the method is far below the maximum limit set by the national standards, with good detection sensitivity.