In this study, salting-out assisted liquid-liquid extraction combined with high performance liquid chromatography diode array detector (SALLE-HPLC-DAD) method was developed and validated for simultaneous analysis of c...In this study, salting-out assisted liquid-liquid extraction combined with high performance liquid chromatography diode array detector (SALLE-HPLC-DAD) method was developed and validated for simultaneous analysis of carbaryl, atrazine, propazine, chlorothalonil, dimethametryn and terbutryn in environmental water samples. Parameters affecting the extraction efficiency such as type and volume of extraction solvent, sample volume, salt type and amount, centrifugation speed and time, and sample pH were optimized. Under the optimum extraction conditions the method was linear over the range of 10 - 100 μg/L (carbaryl), 8 - 100 μg/L (atarzine), 7 - 100 μg/L (propazine) and 9 - 100 μg/L (chlorothalonil, terbutryn and dimethametryn) with correlation coefficients (R2) between 0.99 and 0.999. Limits of detection and quantification ranged from 2.0 to 2.8 μg/L and 6.7 to 9.5 μg/L, respectively. The extraction recoveries obtained for ground, lake and river waters were in a range of 75.5% to 106.6%, with the intra-day and inter-day relative standard deviation lower than 3.4% for all the target analytes. All of the target analytes were not detected in these samples. Therefore, the proposed SALLE-HPLC-DAD method is simple, rapid, cheap and environmentally friendly for the determination of the aforementioned herbicides, insecticide and fungicide residues in environmental water samples.展开更多
建立了液相色谱-串联质谱法定量测定生姜中27种氨基甲酸酯类农药及其代谢物残留的方法.样品用乙腈均质提取,氯化钠盐析分层,氨基固相萃取小柱净化,以乙腈-水（1∶1）为定容溶剂,经Agilent Eclipse Plus C18色谱柱分离,电喷雾串联质谱多...建立了液相色谱-串联质谱法定量测定生姜中27种氨基甲酸酯类农药及其代谢物残留的方法.样品用乙腈均质提取,氯化钠盐析分层,氨基固相萃取小柱净化,以乙腈-水（1∶1）为定容溶剂,经Agilent Eclipse Plus C18色谱柱分离,电喷雾串联质谱多反应监测模式测定,基质匹配标准溶液外标法定量.27种化合物在测定的范围内线性关系良好（r^2 ＞0.99）,方法的检出限为0.05～2.0μg/kg.在加标水平为10、30、100 μg/kg时,方法的回收率为70.9％～119.1％,相对标准偏差为1.0％～10.8％.该方法样品前处理简单、分析时间短、选择性好、灵敏度高,适用于生姜中氨基甲酸酯类农药及其代谢物的快速测定.展开更多
文摘In this study, salting-out assisted liquid-liquid extraction combined with high performance liquid chromatography diode array detector (SALLE-HPLC-DAD) method was developed and validated for simultaneous analysis of carbaryl, atrazine, propazine, chlorothalonil, dimethametryn and terbutryn in environmental water samples. Parameters affecting the extraction efficiency such as type and volume of extraction solvent, sample volume, salt type and amount, centrifugation speed and time, and sample pH were optimized. Under the optimum extraction conditions the method was linear over the range of 10 - 100 μg/L (carbaryl), 8 - 100 μg/L (atarzine), 7 - 100 μg/L (propazine) and 9 - 100 μg/L (chlorothalonil, terbutryn and dimethametryn) with correlation coefficients (R2) between 0.99 and 0.999. Limits of detection and quantification ranged from 2.0 to 2.8 μg/L and 6.7 to 9.5 μg/L, respectively. The extraction recoveries obtained for ground, lake and river waters were in a range of 75.5% to 106.6%, with the intra-day and inter-day relative standard deviation lower than 3.4% for all the target analytes. All of the target analytes were not detected in these samples. Therefore, the proposed SALLE-HPLC-DAD method is simple, rapid, cheap and environmentally friendly for the determination of the aforementioned herbicides, insecticide and fungicide residues in environmental water samples.
