Dos Santos Luciana B O, Infante Carlos M C, Masini Jorge C
Instituto de Química, Universidade de São Paulo, C.P. 26077, São Paulo, SP, Brazil.
J Sep Sci. 2009 Feb;32(4):494-500. doi: 10.1002/jssc.200800563.
This paper describes the development of a sequential injection chromatography (SIC) procedure for separation and quantification of the herbicides simazine, atrazine, and propazine exploring the low backpressure of a 2.5 cm long monolithic C(18) column. The separation of the three compounds was achieved in less than 90 s with resolution >1.5 using a mobile phase composed by ACN/1.25 mmol/L acetate buffer (pH 4.5) at the volumetric ratio of 35:65 and flow rate of 40 microL/s. Detection was made at 223 nm using a flow cell with 40 mm of optical path length. The LOD was 10 microg/L for the three triazines and the quantification limits were of 30 microg/L for simazine and propazine and 40 microg/L for atrazine. The sampling frequency is 27 samples per hour, consuming 1.1 mL of ACN per analysis. The proposed methodology was applied to spiked water samples and no statistically significant differences were observed in comparison to a conventional HPLC-UV method. The major metabolites of atrazine and other herbicides did not interfere in the analysis, being eluted from the column either together with the unretained peak, or at retention times well-resolved from the studied compounds.
本文描述了一种顺序注射色谱法（SIC）的开发过程，该方法利用一根2.5 cm长的整体式C(18)柱的低背压来分离和定量除草剂西玛津、莠去津和扑灭津。使用由乙腈/1.25 mmol/L醋酸盐缓冲液（pH 4.5）组成的流动相，体积比为35:65，流速为40 μL/s，在不到90秒内实现了三种化合物的分离，分离度>1.5。使用光程长度为40 mm的流通池在223 nm处进行检测。三种三嗪类化合物的检测限为10 μg/L，西玛津和扑灭津的定量限为30 μg/L，莠去津的定量限为40 μg/L。采样频率为每小时27个样品，每次分析消耗1.1 mL乙腈。将所提出的方法应用于加标水样，与传统的HPLC-UV方法相比，未观察到统计学上的显著差异。莠去津和其他除草剂的主要代谢产物在分析中不产生干扰，它们要么与未保留的峰一起从柱中洗脱，要么在与所研究化合物保留时间良好分离的位置洗脱。
