提出了测定水中呋喃丹和甲萘威的柱后衍生-高效液相色谱法。水样经盐酸酸化至pH 3后,用0.45 μm水性滤膜过滤,取200 μL水样直接进样,用Waters Carbamate Analysis分析柱(3.9 mm×150 mm,5 μm)和以甲醇-乙腈-水(1+1+3)混合液作为流动相进行分离。分离后用2 g·L-1氢氧化钠溶液进行水解,用每升中含邻苯二甲醛0.1 g、十水硼酸钠19.1 g及2-巯基乙醇0.5 mL的溶液进行衍生化,用荧光检测器在激发波长(λex)为339 nm,发射波长(λem)为445 nm处检测。方法检出限(3S/N)均为4×10-4 mg·L-1。应用此方法测定了水厂出厂水和河水中呋喃丹和甲萘威,并用标准加入法做回收试验,测得其平均回收率依次为93.0%~98.0%之间和93.0%~99.4%之间,相对标准偏差(n=6)小于0.50%。

HPLC was applied to the determination of the insecticides carbofuran and carbaryl in water with post-derivatization. The water sample was adjusted to pH 3 with HCl and filtered with hydrophilic filtering membrane of 0.45 μm. 200 μL of the filtrate was taken for HPLC analysis. Waters Carbamate Analysis column (3.9 mm×150 mm, 5 μm) and mobile phase of a mixture of methanol-acetonitrile-H2O (1+1+3) were used in the separation. The eluate was hydrolyzed with 2 g·L-1 NaOH solution and derivatized with a solution containing 0.1 g phthaldehyde, 19.1 g of sodium borate (10 hydrate) and 0.5 mL of 2 mercaptoethanol per liter of the solution. Fluorescence detection was made at λex 339 nm and λem 445 nm. Detection limits (3S/N) found were same as 4×10-4mg·L-1 for both the insecticides. Samples of tap water and river water were analyzed by the proposed method and recovery was tested by addition of standards, values of recovery found were in the ranges of 93.0%-98.0% (for carbofuran) and 93.0%-99.4% (for carbaryl) with values of RSD′s (n=6) less than 0.50%.