土壤、水和小麦中除草剂氯氟吡氧乙酸残留检测前处理方法

Preparation of Starane Residues Determination in Soil, Water and Wheat

建立了高效液相色谱(HPLC)法测定水、土壤和小麦中除草剂氯氟吡氧乙酸残留量的分析方法。水样直接用LC-18固相萃取小柱分离、净化和富集;采用乙酸乙酯/石油醚(体积比2∶1)振荡提取,磺化法净化,测定土壤中氯氟吡氧乙酸残留量;以乙腈/水(体积比4∶1)为提取剂,氟罗里硅土固相萃取小柱分离、净化,测定小麦样品中氯氟吡氧乙酸的残留量。结果表明:HPLC法检测氯氟吡氧乙酸的线性范围为0.5～20.0mg/L,决定系数r2=0.9997,最低检测质量浓度为0.01mg/L。水样的加标回收率为91.8%～93.9%,相对标准偏差为0.7%～1.2%;土壤的加标回收率为90.1%～94.1%,相对标准偏差为1.0%～1.9%;小麦的加标回收率为93.5%～94.9%,相对标准偏差为4.2%～5.4%。

A method for determination of herbicide starane in water, soil and wheat by high-performance liquid chromatography （HPLC） was developed. Water samples were extracted and purified and collected by solid-phase extraction （SPE） LC-18 column. Soil samples were extracted by ethyl acetate/petroleum ether（2：1, by vol） and purified by sulphonation. Wheat sample was extracted by acetonitrile/water（4：1, by vol） and purified and collected by SPE- Florisil column. The calibration curves of the method were determined in the range of 0.5 to 20.0 mg/L, with the correlation coefficients （r^2） was 0.9997 with the minimal detection limits being 0.01 mg/L. The spiked recoveries of water sample ranged from 91.8 to 93.9%, the soil sample for 90.1 to 94.1%, the wheat sample for 93.5 to 94.9%, with the relative standard deviations （RSD） were from 0.7 to 1.2%, 1.0 to 1.9% and 4.2 to 5.4% respectively.