Chromatographia ( IF 1.7 ) Pub Date : 2023-08-16 , DOI: 10.1007/s10337-023-04274-z Hiago de Oliveira Gomes , Ellen Cristine Lopes da Silva Bento , Clenel Robson Feitosa dos Santos , Roseni da Silva Cardoso , Carliane de Oliveira de Souza , Ligia Claudia Castro de Oliveira , José Galberto Martins da Costa , Ronaldo Ferreira do Nascimento , Raimundo Nonato Pereira Teixeira
In this study, the efficiency of two detectors—variable wavelength detector (VWD) and fluorescence detector (FLD)—in a liquid chromatograph to quantify azoxystrobin in water was compared. For this, a method was developed in a HPLC-VWD-FLD system using extraction by modified QuEChERS. The detection of azoxystrobin by fluorescence was possible using only a solvent effect, considering that azoxystrobin does not naturally fluoresce. Analytical curves were constructed using matrix-matched calibration, where a low matrix effect was verified in both detectors. In the linearity analysis of the analytical curves, the values of coefficient of determination found for the detectors were 0.9989 and 0.9983 for VWD and FLD, respectively. The relative standard error for the VWD detector was 6.96%, while for the fluorescence detector, it was 5.49%. The limit of detection (LOD) and the limit of quantification (LOQ) were, respectively, 0.33 and 0.68 mg L−1 (VWD) and 0.18 and 0.37 mg L−1 (FLD). The QuEChERS method, originally developed for the extraction of pesticides in food, was adapted for the extraction of azoxystrobin in water, demonstrating efficiency in the process, with precision values lower than 20% and accuracy between 83.58 and 112.88%, within the criteria established by MAPA and Document Nº SANTE/11312/2021. Therefore, it is concluded that both detectors are suitable for the analysis of azoxystrobin in water; however, there is a greater sensitivity for the fluorescence detector, since lower detection and quantification limit values were observed, in addition to a lower standard relative error (RSE).
中文翻译:
HPLC 系统中 VWD 和 FLD 检测器定量水中嘧菌酯的比较研究
在本研究中,比较了液相色谱仪中两种检测器(可变波长检测器 (VWD) 和荧光检测器 (FLD))对水中嘧菌酯定量的效率。为此,我们在 HPLC-VWD-FLD 系统中开发了一种使用改进的 QuEChERS 萃取的方法。考虑到嘧菌酯本身不发出荧光,仅利用溶剂效应就可以通过荧光检测嘧菌酯。使用基质匹配校准构建分析曲线,在两个探测器中验证了低基质效应。在分析曲线的线性分析中,发现VWD和FLD探测器的决定系数值分别为0.9989和0.9983。VWD检测器的相对标准误差为6.96%,而荧光检测器的相对标准误差为5.49%。−1 (VWD) 以及 0.18 和 0.37 mg L −1 (FLD)。QuEChERS 方法最初是为食品中农药的提取而开发的,后来适用于水中嘧菌酯的提取,证明了该过程的效率,精度值低于 20%,准确度在 83.58 至 112.88% 之间,符合标准由 MAPA 和文件号 SANTE/11312/2021 建立。因此,两种检测器均适用于水中嘧菌酯的分析;然而,荧光检测器的灵敏度更高,因为除了较低的标准相对误差 (RSE) 之外,还观察到较低的检测和定量限值。