Geerdink R B, Graumans A M, Viveen J
Institute for Inland Water Management and Waste Water Treatment, AA Lelystad, Netherlands.
J Chromatogr. 1991 Jun 28;547(1-2):478-83. doi: 10.1016/s0021-9673(01)88676-3.
Novel clean-up techniques for a polymeric precolumn (PLRP-S) for the subsequent determination of bentazone and eight phenoxy acid herbicides in surface water samples are described. After preconcentration of the components at pH 3 on a 10 x 2 mm I.D. precolumn, the technique consists of a clean-up with 1000 microliters of 0.1 mol/l sodium hydroxide solution (pH 12.5) and of a heartcut consisting of four precolumn bed volumes of eluent directed to waste followed by ten precolumn bed volumes of eluent directed to the analytical column. Analytical separation is performed with acetonitrile-water (30:70) containing 0.005 mol/l of tetrabutylammonium hydrogensulphate (pH 8.3) (which is also the desorption eluent during heartcutting) on a polymeric analytical column (PLRP-S). With 25 ml of surface water, spiked at 0.25 and 1 microgram/l, applied to the precolumn, recoveries for all components were over 85% with a relative standard deviation (n = 5) of ca. 9% at 0.25 microgram/l and ca. 2% at 1 microgram/l. Detection limits in surface water samples are 0.05-0.1 microgram/l. Owing to automation, the total analysis time is ca. 30 min.
本文描述了一种用于聚合物预柱(PLRP-S)的新型净化技术,该技术用于后续测定地表水样中的苯达松和八种苯氧羧酸类除草剂。在pH为3的条件下,将组分在10×2 mm内径的预柱上进行预富集后,该技术包括用1000微升0.1 mol/L氢氧化钠溶液(pH 12.5)进行净化,以及一次中心切割,即先将四个预柱床体积的洗脱液导向废液,然后将十个预柱床体积的洗脱液导向分析柱。在聚合物分析柱(PLRP-S)上,使用含有0.005 mol/L硫酸氢四丁铵(pH 8.3)的乙腈-水(30:70)(这也是中心切割过程中的解吸洗脱液)进行分析分离。将25 ml分别加标至0.25和1微克/升的地表水样品应用于预柱,所有组分的回收率均超过85%,在0.25微克/升时相对标准偏差(n = 5)约为9%,在1微克/升时约为2%。地表水样中的检测限为0.05 - 0.1微克/升。由于实现了自动化,总分析时间约为30分钟。