| 新型柱前衍生试剂分析草甘膦的高效液相色谱研究 |
| |
| 引用本文： | 方芳,;魏荣卿,;刘晓宁,;李寿椿.新型柱前衍生试剂分析草甘膦的高效液相色谱研究[J].生物加工过程,2014(3):69-72. |
| |
| 作者姓名： | 方芳 ;魏荣卿 ;刘晓宁 ;李寿椿 |
| |
| 作者单位： | [1]南京工业大学生物与制药工程学院,南京211800; [2]南京中意化工技术开发研究所,南京210009 |
| |
| 基金项目： | 国家高技术研究发展计划（863计划）项目（2007AA022200,2007AA06A402） |
| |
| 摘 要： | 以2,5-二甲氧基苯磺酰氯(DMOSC)为柱前衍生化试剂,建立了柱前衍生草甘膦的紫外检测反相高效液相色谱法,并优化了衍生化条件,得最佳条件:衍生温度35℃,时间15 min,pH 10.0,草甘膦与DMOSC的摩尔比为1∶6。HPLC分析条件:采用Kromasil C18柱,流速1.0 mL/min,柱温30℃,检测波长220 nm,流动相为甲醇-乙腈-磷酸盐缓冲溶液(0.02 mol/L、pH 5.5),三者的体积比为15∶5∶80。结果表明:草甘膦质量浓度在5~100μg/mL范围内线性关系良好,相关系数为0.996 2,检测限为0.067μg/mL。实验表明该方法反应条件温和,灵敏度高,衍生产物稳定。
|
| 关 键 词： | 衍生 -二甲氧基苯磺酰氯 草甘膦 高效液相色谱 |
Determination of glyphosate by HPLC with a novel pre-column derivatization reagent |
| |
| Affiliation: | FANG Fang, WEI Rongqing, LIU Xiaoning, LI Shouchun ( 1. College of Biotechnology and Pharmaceutical Engineering, Nanjing Tech University, Nanjing 211800, China; 2. Sino Italian Chemitech R＆D Institute,Nanjing 210009,China) |
| |
| Abstract: | A derivatization method for the determination of glyphosate had been developed by using 2,5-dimethoxybenzenesulfonyl chloride.The optimized conditions of derivatization were as follows：reaction temperature 35 ℃,reaction time 15 min,solution pH value 10.0,the buffer reaction concentration 0.2 mol/L,and ratio of n（ glyphosate） ∶n（ o-nitrobenzenesulfonyl）= 1∶6.The chromatographic conditions were as follows：Kromasil C18 column（5 μm,4.6 ＆#215;250 mm）,detection wavelength 220 nm,flow rate 1.0 mL/min,mobile phase A （ methanol）∶mobile phase B （ acetonitrile）∶mobile phase C （ phosphate buffer solution（PBS,pH 5.5,0.02 mol/L））= 15∶5∶80,isocratic elution.The calibration curve for glyphosate was linear ranging from 5 μg/mL to 100 μg/mL. The linear correlation coefficient was 0.996 2. The limit of detection was 0.067 μg/mL.The experimental result shows that the method is simple,rapid and reliable,and generally applicable. |
| |
| Keywords: | derivatization 2 5-dimethoxybenzenesulfonyl chloride glyphosate HPLC |
| 本文献已被 CNKI 维普 等数据库收录！ |
|
