Sun Lisi, Kong Deyang, Gu Weidong, Guo Xinyan, Tao Wenqi, Shan Zhengjun, Wang Ying, Wang Na
Nanjing Institute of Environmental Sciences, Ministry of Environmental Protection, Nanjing, China; Key Laboratory of Pesticide Environmental Assessment and Pollution Control, Ministry of Environmental Protection of China, Nanjing, China; School of Chemical Engineering, Nanjing University of Science and Technology, Nanjing, China.
Nanjing Institute of Environmental Sciences, Ministry of Environmental Protection, Nanjing, China; Key Laboratory of Pesticide Environmental Assessment and Pollution Control, Ministry of Environmental Protection of China, Nanjing, China.
J Chromatogr A. 2017 Jun 16;1502:8-13. doi: 10.1016/j.chroma.2017.04.018. Epub 2017 Apr 12.
In order to evaluate the pollution caused due to glyphosate (Glyp) in soils and sludge, it is important to establish a set of standard determination techniques. In this work, the previously reported HPLC analytical method for determination of Glyp has been improved in order to be applied for all kinds of soils/sludge. The soil/sludge samples were extracted using sodium phosphate and trisodium citrate aqueous solutions. The extract was adjusted to pH 9 and contaminations were removed by washing with n-hexane. The method developed in this work further involves derivatization with 9-fluorenylmethylchloroformate (FMOC-Cl) followed by high performance liquid chromatography (HPLC) coupled with fluorescence detection. The method was validated in three soil (red soil, black soil and paddy soil) and two sludge samples (lake and river sludge) from China and verified in six laboratories. A good linear relationship (correlation coefficients ≥0.999) was observed within the range of 0.005-0.5mg/L. The limit of detection (LOD) and the limit of quantitation (LOQ) were determined to be 0.01mg/kg and 0.04mg/kg, respectively. The precision and accuracy were satisfactory with the relative standard deviation (RSD) lower than 15% and the mean recovery values ranging from 75% to 110% (n=6), that spiked at three levels (0.1, 0.5 and 1.0mg/kg).
为了评估草甘膦（Glyp）对土壤和污泥造成的污染，建立一套标准测定技术很重要。在本研究中，对先前报道的测定Glyp的高效液相色谱（HPLC）分析方法进行了改进，以便应用于各类土壤/污泥。土壤/污泥样品用磷酸钠和柠檬酸三钠水溶液进行提取。将提取物调节至pH 9，并用正己烷洗涤以去除污染物。本研究开发的方法进一步包括用9-芴基甲基氯甲酸酯（FMOC-Cl）进行衍生化，然后进行高效液相色谱（HPLC）结合荧光检测。该方法在中国的三种土壤（红壤、黑壤和水稻土）和两种污泥样品（湖泊和河流污泥）中进行了验证，并在六个实验室进行了核查。在0.005 - 0.5mg/L范围内观察到良好的线性关系（相关系数≥0.999）。检测限（LOD）和定量限（LOQ）分别确定为0.01mg/kg和0.04mg/kg。在三个加标水平（0.1、0.5和1.0mg/kg）下，精密度和准确度令人满意，相对标准偏差（RSD）低于15%，平均回收率在75%至110%之间（n = 6）。
