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    自动固相萃取-超高效液相色谱-柱后衍生法测定水中呋喃丹的含量

    UHPLC Determination of Carbofuran in Water with Automatic SPE and Post Column Derivatization

    • 摘要: 采用自动固相萃取-超高效液相色谱-柱后衍生法测定水中呋喃丹的含量。水样(200 mL)以5 mL·min-1流量富集于C18 SPE小柱上,用吹氮法吹干小柱,用四氢呋喃5 mL,以1 mL·min-1流量洗脱,所得洗脱液吹氮至近干,用甲醇定容至1 mL。试液按色谱分离条件操作,所得洗脱液[甲醇-水(60+40)]进行柱后衍生反应单元。用2.0 g·L-1氢氧化钠溶液为水解试剂,以邻苯二甲醛荧光试剂溶液为衍生试剂,上述两者的流量均为0.3 mL·min-1,水解温度为105 ℃,对所得衍生物进行荧光检测(λex=339 nm,λem=445 nm)。呋喃丹的质量浓度在0.010~2.00 mg·L-1范围内与其峰面积呈线性关系。方法的检出限(3S/N)为0.87 μg·L-1,加标回收率在99.3%~100%之间,测定值的相对标准偏差(n=6)均小于3.5%。

       

      Abstract: UHPLC with post-column derivatization after enrichment by automatic SPE was applied to the determination of carbofuran (CFR) in water. The water sample (200 mL) was passed through C18 SPE micro-column at a flow rate of 5 mL·min-1. The column was then dried by N2-blowing and eluted with 5 mL of tetrahydrofuran at a flow rate of 1 mL·min-1. The eluate was evaporated to near-dryness by N2-blowing,and the concentrate was dissolved and made up to 1 mL with methanol. Chromatographic separation was made with the sample solution according to the prscribed chromatographic conditions,and the eluate in the mobile phase of CH3OH-H2O (60+40) mixture was led to the post-derivatization unit,where hydrolysis and derivatization were carried out by using 2.0 g·L-1 NaOH solution as hydrolyzing reagent and a solution of o-benzenediformaldehyde in sadium borate solution as derivatizing agent flowing at a same rate of 0.3 mL·min-1,at a hydrolysis temperature of 105 ℃. Intensity of fluorescence of the derivate was measured at λex of 339 nm and λem of 445 nm. Linear relationships between values of peak area and mass concentration of CFR was obtained in the range of 0.010-2.00 mg·L-1,with detection limit (3S/N) of 0.87 μg·L-1. Values of recovery found by standard addition method were in the range of 99.3%-100%. Values of RSD′s (n=6) found were all less than 3.5%.

       

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