建立了超高效液相色谱-串联四极杆复合线性离子阱质谱(Ultra performance liquid chromatographytriple quadrupole-linear ion trap mass spectrometry,UPLC-QTRAP)技术结合QuEChERS(Quiek,Easy,Cheap,Effective,Rugged,and Safe)法检...建立了超高效液相色谱-串联四极杆复合线性离子阱质谱(Ultra performance liquid chromatographytriple quadrupole-linear ion trap mass spectrometry,UPLC-QTRAP)技术结合QuEChERS(Quiek,Easy,Cheap,Effective,Rugged,and Safe)法检测尿样中毒死蜱代谢产物残留的分析方法。采用乙腈提取,PSA和BCB净化,ZORBAX Eclipse Plus C18色谱柱分离,以乙腈-0.2%氨水为流动相梯度洗脱,在电喷雾电离(ESI负离子模式下),使用触发增强子离子扫描方式(MRM-IDA-EPI)对尿样中毒死蜱的代谢产物进行定性和定量分析。方法线性范围为1.0~100.0μg/L,检出限0.10~0.73μg/L。尿样中3种毒死蜱代谢物的平均加标回收率在80.3%~90.1%之间,RSD均小于5%。本方法操作简单、灵敏度高、准确性好、重现性强,利用QTRAP的质谱优势可有效的对色谱峰进行鉴定,有效预防样品的假阳性。本方法已成功应用于人体尿液实际样品中,检出的浓度范围为ND^54.6μg/L。本方法可为复杂基质中化学品的识别和定量提供技术参考。展开更多
Response of two wheat cultivars （Triticum aestivum cv. YM 158 and NM 9） to the herbicide chlorotoluron and the effect of two forms of dissolved organic matter on the chlorotoluron toxicity to the plants were charact...Response of two wheat cultivars （Triticum aestivum cv. YM 158 and NM 9） to the herbicide chlorotoluron and the effect of two forms of dissolved organic matter on the chlorotoluron toxicity to the plants were characterized. Treatment with chlorotoluron at 10-50 μg/ml inhibited the seed germination and a dose-response was observed. The inhibition of seed germination was correlated to the depression of a-amylase activities. To identify whether chlorotoluron induced oxidative damage to wheat plants, the malondlaldehyde （MDA） content and electrolyte leakage were measured. Results showed that both MDA content and electrolyte leakage in the chlorotoluron-treated roots significantly increased. Activities of several key enzymes were measured that operate in citric acid cycle and carbohydrate metabolic pathway. Inhibited activities of citrate synthase and NADP-isocitrate dehydrogenase were observed in the chlorotoluron-treated roots as compared to control plants. We also examined malate dehydrogenase and phosphoenolpyruvate carboxylase in wheat roots exposed to 30 μg/ml chlorotoluron, liowever, none of the enzymes showed significant changes in activities. Application of 160 μg/ml dissolved organic matter （DOM） extracted from non-treated sludge（NTS） and heat-expanded sludge （lIES） in the medium with 30 μg/ml chlorotoluron induced an additive inhibition of seed germination and plant growth. The inhibition of growth due to the DOM treatment was associated with the depression of activities of a-amylase, citrate synthase and NADP-isocitrate dehydrogenase, as well as the increase in malondlaldehyde content and electrolyte leakage. These results suggested that the presence of DOM might enhance the uptake and accumulation of chlorotoluron, and thus resulted in greater toxicity in wheat plants. The two forms of DOM exhibited differences in regulation of chlorotoluron toxicity to the wheat plants. Treatments with DOM-NTS induced greater toxicity to plants as compared to those with DOM-HES. In addition to DOM affecting chlorotoluron-induced toxicity to wheat plants, the cultivars could have also contributed to differences. Generally, NM-9 showed a higher sensitivity to chlorotoluron than YM 158 either in the absence or in the presence of DOM.展开更多
文摘建立了超高效液相色谱-串联四极杆复合线性离子阱质谱(Ultra performance liquid chromatographytriple quadrupole-linear ion trap mass spectrometry,UPLC-QTRAP)技术结合QuEChERS(Quiek,Easy,Cheap,Effective,Rugged,and Safe)法检测尿样中毒死蜱代谢产物残留的分析方法。采用乙腈提取,PSA和BCB净化,ZORBAX Eclipse Plus C18色谱柱分离,以乙腈-0.2%氨水为流动相梯度洗脱,在电喷雾电离(ESI负离子模式下),使用触发增强子离子扫描方式(MRM-IDA-EPI)对尿样中毒死蜱的代谢产物进行定性和定量分析。方法线性范围为1.0~100.0μg/L,检出限0.10~0.73μg/L。尿样中3种毒死蜱代谢物的平均加标回收率在80.3%~90.1%之间,RSD均小于5%。本方法操作简单、灵敏度高、准确性好、重现性强,利用QTRAP的质谱优势可有效的对色谱峰进行鉴定,有效预防样品的假阳性。本方法已成功应用于人体尿液实际样品中,检出的浓度范围为ND^54.6μg/L。本方法可为复杂基质中化学品的识别和定量提供技术参考。
基金The National Natural Science Foundation of China（30170537）
文摘Response of two wheat cultivars （Triticum aestivum cv. YM 158 and NM 9） to the herbicide chlorotoluron and the effect of two forms of dissolved organic matter on the chlorotoluron toxicity to the plants were characterized. Treatment with chlorotoluron at 10-50 μg/ml inhibited the seed germination and a dose-response was observed. The inhibition of seed germination was correlated to the depression of a-amylase activities. To identify whether chlorotoluron induced oxidative damage to wheat plants, the malondlaldehyde （MDA） content and electrolyte leakage were measured. Results showed that both MDA content and electrolyte leakage in the chlorotoluron-treated roots significantly increased. Activities of several key enzymes were measured that operate in citric acid cycle and carbohydrate metabolic pathway. Inhibited activities of citrate synthase and NADP-isocitrate dehydrogenase were observed in the chlorotoluron-treated roots as compared to control plants. We also examined malate dehydrogenase and phosphoenolpyruvate carboxylase in wheat roots exposed to 30 μg/ml chlorotoluron, liowever, none of the enzymes showed significant changes in activities. Application of 160 μg/ml dissolved organic matter （DOM） extracted from non-treated sludge（NTS） and heat-expanded sludge （lIES） in the medium with 30 μg/ml chlorotoluron induced an additive inhibition of seed germination and plant growth. The inhibition of growth due to the DOM treatment was associated with the depression of activities of a-amylase, citrate synthase and NADP-isocitrate dehydrogenase, as well as the increase in malondlaldehyde content and electrolyte leakage. These results suggested that the presence of DOM might enhance the uptake and accumulation of chlorotoluron, and thus resulted in greater toxicity in wheat plants. The two forms of DOM exhibited differences in regulation of chlorotoluron toxicity to the wheat plants. Treatments with DOM-NTS induced greater toxicity to plants as compared to those with DOM-HES. In addition to DOM affecting chlorotoluron-induced toxicity to wheat plants, the cultivars could have also contributed to differences. Generally, NM-9 showed a higher sensitivity to chlorotoluron than YM 158 either in the absence or in the presence of DOM.
