Charoenkitamorn Kanokwan, Chailapakul Orawon, Siangproh Weena
Electrochemistry and Optical Spectroscopy Research Unit, Department of Chemistry, Faculty of Science, Chulalongkorn University, 254 Phayathai Road, Patumwan, Bangkok 10330, Thailand.
Electrochemistry and Optical Spectroscopy Research Unit, Department of Chemistry, Faculty of Science, Chulalongkorn University, 254 Phayathai Road, Patumwan, Bangkok 10330, Thailand; National Center of Excellent of Petroleum, Petrochemicals and Advanced Materials, Chulalongkorn University, Patumwan, Bangkok 10330, Thailand.
Talanta. 2015 Jan;132:416-23. doi: 10.1016/j.talanta.2014.09.020. Epub 2014 Sep 30.
For the first time, gold nanoparticles (AuNPs) modified screen-printed carbon electrode (SPCE) was developed as working electrode in ultra-high performance liquid chromatography (UHPLC) coupled with electrochemical detection (UHPLC-ED) for simultaneous determination of thiram, disulfiram, and N,N-diethyl-N',N'-dimethylthiuram disulfide, their derivative compound. The separation was performed in reversed-phase mode using C18 column, mobile phase consisting of 55:45 (v/v) ratio of 0.05 M phosphate buffer solution (pH 5) and acetonitrile at a flow rate of 1.5 mL min(-1). For the detection part, the amperometric detection was chosen with a detection potential of 1.2 V vs. Ag/AgCl. Under the optimal conditions, the good linear relationship was obtained in the range of 0.07-15, 0.07-12, and 0.5-15 µg mL(-1) (correlation coefficient more than 0.9900) for thiram, N,N-diethyl-N',N'-dimethylthiuram disulfide, and disulfiram, respectively. The limits of detection (LODs) of thiram, N,N-diethyl-N',N'-dimethylthiuram disulfide, and disulfiram were 0.022, 0.023, and 0.165 µg mL(-1), respectively. Moreover, this method was successfully applied for the detection of these compounds in real samples (apple, grape and lettuce) with the recoveries ranging from 94.3% to 108.8%. To validate this developed method, a highly quantitative agreement was clearly observed compared to standard UHPLC-UV system. Therefore, the proposed electrode can be effectively used as an alternative electrode in UHPLC-ED for rapid, selective, highly sensitive, and simultaneous determination of thiram, disulfiram, and N,N-diethyl-N',N'-dimethylthiuram disulfide.
首次将金纳米颗粒(AuNPs)修饰的丝网印刷碳电极(SPCE)开发为超高效液相色谱(UHPLC)结合电化学检测(UHPLC-ED)中的工作电极,用于同时测定福美双、双硫仑及其衍生物N,N-二乙基-N',N'-二甲基秋兰姆二硫化物。分离在反相模式下使用C18柱进行,流动相由体积比为55:45的0.05 M磷酸盐缓冲溶液(pH 5)和乙腈组成,流速为1.5 mL min(-1)。对于检测部分,选择安培检测,检测电位为相对于Ag/AgCl为1.2 V。在最佳条件下,福美双、N,N-二乙基-N',N'-二甲基秋兰姆二硫化物和双硫仑分别在0.07 - 15、0.07 - 12和0.5 - 15 µg mL(-1)范围内获得了良好的线性关系(相关系数大于0.9900)。福美双、N,N-二乙基-N',N'-二甲基秋兰姆二硫化物和双硫仑的检测限(LOD)分别为0.022、0.023和0.165 µg mL(-1)。此外,该方法成功应用于实际样品(苹果、葡萄和生菜)中这些化合物的检测,回收率在94.3%至108.8%之间。为了验证该开发方法,与标准UHPLC-UV系统相比,明显观察到高度定量的一致性。因此,所提出的电极可有效地用作UHPLC-ED中的替代电极,用于快速、选择性、高灵敏度地同时测定福美双、双硫仑和N,N-二乙基-N',N'-二甲基秋兰姆二硫化物。