【摘要】 采用在线柱浓缩-超高效液相色谱联用技术测定水体中痕量甲萘威和呋喃丹。水样过滤后直接进样,采用固相萃取小柱富集待测物,梯度洗脱后,利用阀切换技术将待测物反冲至分析柱Acclaim RSLC C18(100 mm×2.1mm,2.2μm)上进行色谱分离,以10 mmo l/L醋酸铵缓冲溶液(pH 5.0,用醋酸调节)和乙腈分别为流动相A和B,梯度洗脱,泵流速为0.8 mL/min,检测波长为280 nm,二极管阵列检测器检测。甲萘威和呋喃丹在1.0～100μg/L范围内线性良好(相关系数r2>0.999 9),检出限(S/N=3)分别为0.5和0.25μg/L,加标回收率为76.0%～120.0%。用所建立的方法测定了水中痕量的甲萘威与呋喃丹的含量,结果令人满意。更多还原

【Abstract】 An online column enrichment-ultra high performance liquid chromatography(UHPLC) method was developed to determine trace carbaryl and carbofuran in water.The sample was injected into a UHPLC system directly after filtration with 0.22 μm membrane,and then enriched by online solid phase extraction(SPE) column.The analyte was back-flushed into the analytical column Acclaim RSLC C18(100 mm×2.1 mm,2.2 μm) by valve switching method.The mobile phases were 10 mmol/L ammonium acetate buffer(pH 5.0,adjusted by acetic acid) and acetonitrile in a gradient elution mode with a flow rate of 0.8 mL/min,and detected by a diode array detector with the detection wavelength of 280 nm.The good linear ranges of carbaryl and carbofuran were 1.0-100 μg/L with the correlation coefficients(r2) larger than 0.999 9,and the limits of detection(S/N=3) were 0.5 μg/L and 0.25 μg/L,respectively.The average spiked recoveries were in the range of 76.0%-120.0%.The method has been applied to determine trace carbaryl and carbofuran in water samples with satisfactory results.更多还原