三氟苯嘧啶在水稻、土壤和田水中的残留分析方法

Analysis of Triflumezopyrim Residues in Rice, Soil and Field Water

[目的]建立高效液相色谱法检测水稻(糙米、谷壳和植株)、土壤和田水中三氟苯嘧啶残留的方法。[方法]待测样品中的三氟苯嘧啶用乙腈提取,糙米、植株和谷壳用PSA及Carbon-GCB吸附剂分散固相萃取净化,高效液相色谱检测,外标法定量。[结果]方法的线性范围为0.1~20 mg/L,相关系数为0.9999;在0.05、0.2、1 mg/kg 3个添加水平下,糙米和土壤中的平均回收率分别为84.3%~98.4%和80.1%~96.2%,相对标准偏差分别为2.52%~8.9%和3.33%~7.41%。在0.1、1、5 mg/kg 3个添加水平下,植株和稻壳的平均回收率分别为90.1%~99.8%和93.5%~96.1%,相对标准偏差分别为1.56%~8.31%和4.29%~6.77%。在0.02、0.2、1 mg/kg 3个添加水平下,田水的平均回收率为81.5%~95.2%,相对标准偏差为3.39%~7.78%。在上述检测条件下,三氟苯嘧啶的最小检出量为2 ng。[结论]该方法简单可靠,灵敏度、准确度、精密度符合农药残留分析要求,可用于水稻、土壤和田水中三氟苯嘧啶的残留检测。

[Aims] A new method for analysis of triflumezopyrim residues in rice（rough rice, plant and hull）, soil and field water by high performance liquid chromatograph was developed. [Methods] The samples were extracted with dichloromethane. The triflumezopyrim residues in rough rice, plant and hull were purified by PSA and Carbon-GCB,then separated with SHIMADZU LC-20 AT. Finally, the samples were detected by photodiode array detector of HPLC.[Results] The linear range of calibration curves was 0.1-20 mg/L and linear correlation coefficient was 0.9999. When the spiked levels were 0.05, 0.2 and 1.0 mg/L, the average recoveries of triflumezopyrimin in rough rice were 84.3-98.4%with relative standard deviations of 2.52-8.9%, the average recoveries of triflumezopyrim in soil were 80.1-96.2% with relative standard deviations of 3.33-7.41%. When the spiked levels were 0.1, 1.0 and 5.0 mg/kg, the average recoveries of triflumezopyrim in rice plant were 90.1-99.8% with relative standard deviations of 1.56-8.31%. The average recoveries of triflumezopyrim in rice hull were 93.5-96.1% with relative standard deviations of 4.29-6.77%. When the spiked levels were 0.02, 0.2 and 1.0 mg/kg, the average recoveries of triflumezopyrim in field water were 81.5-95.2%with relative standard deviations of 3.39-7.78%. Under these conditions, the limits of detection for triflumezopyrim were2.0 ng. [Conclusions] The method is simple and reliable, the sensitivity and precision meet with the requirement for pesticide residue analysis, which can be applied for analysis of triflumezopyrim residues in rice, soil and field water.