直接进样或固相萃取-高效液相色谱法测定水中苯菌灵和多菌灵  

Determination of Benomyl and Carbendazim in Water Sample by Direct Injection or Solid Phase Extraction and High Performance Liquid Chromatography

作　　者：熊杰 胥倩 曹阳 何吉明 王若男 XIONG Jie;XU Qian;CAO Yang;HE Jiming;WANG Ruonan(Ecology and Environmental Monitoring of Sichuan,Chengdu 610091,China)

机构地区：[1]四川省生态环境监测总站,四川成都610091

出　　处：《中国环境监测》2023年第1期206-215,共10页Environmental Monitoring in China

基　　金：国家生态环境标准项目(2008-940)。

摘　　要：建立了采用直接进样和固相萃取两种前处理方式,利用高效液相色谱法分析水中苯菌灵和多菌灵的方法。采用0.22μm聚醚砜滤膜过滤样品,或使用C18固相萃取小柱对样品进行前处理后,以C18反相柱为色谱柱,将柱温设定为40℃,流速设定为0.7 mL/min,以甲醇和水为流动相,利用等度洗脱进行分离,使用二极管阵列检测器进行定量,检测波长为280 nm。将苯菌灵在酸性条件下(pH<2.0)静置至少11 h后,转化为多菌灵进行检测。在上述条件下,采取直接进样时,多菌灵的检出限为4μg/L;采用固相萃取进行前处理且水样体积为100 mL时,多菌灵的检出限为0.09μg/L。标准曲线绘制结果显示,该方法在0.02~10.0 mg/L浓度范围内线性良好(r>0.999)。在直接进样条件下测试低、中、高3种浓度的实际水样加标样品,得到的相对标准偏差在0.7%~2.9%之间,回收率在93.5%~102%之间;采用固相萃取时,低、中、高3种浓度的实际加标样品的相对标准偏差在1.3%~4.7%之间,回收率在86.8%~107%之间。测试结果表明,该方法可应用于实际监测工作。A new method was developed for determination of benomyl and carbendazim in water sample by direct injection or solid phase extraction-high performance liquid chromatography(SPE-HPLC).Water sample was cleaned by 0.22μm millipore filter or solid phase extraction(SPE).Chromatographic separation was performed on C18 reversed phase column,the chromatographic conditions as follows:column temperature was 40℃,flow rate was 0.7 mL/min,used methanol and water as mobile phases,separated by isometric elution,and quantified by diode array detector at 280 nm.Benomyl was converted into carbendazim for detection after standing for at least 11 hours under acidic conditions(pH<2.0).Under these conditions,the detection limit of carbendazim was 4μg/L by direct injection,the detection limit of carbendazim was 0.09μg/L by SPE.The calibration curve showed good linearity over the tested range from 0.02 to 10.0 mg/L(r>0.999).The relative standard deviation were 0.7%-2.9%,the recovery rates were 93.5%-102%by direct injection;the relative standard deviation were 1.3%-4.7%,the recovery rates were 86.8%-107%by SPE.Precision and accuracy all met the demands of quality control.The proposed method was successfully applied to determine actual water samples and therefore can be used for environmental monitoring.

关 键 词：苯菌灵 多菌灵 水样 直接进样 固相萃取 高效液相色谱 

分 类 号：X830.2[环境科学与工程—环境工程]