摘要
本研究建立了测定渔业水质中氟乐灵、二甲戊灵、甲草胺、乙草胺、丁草胺、西玛津、莠去津、扑草净8种除草剂残留量的气相色谱-质谱法。样品用氯化钠调节盐度至20-30,二氯甲烷提取,无水硫酸钠除水,过弗罗里硅土固相萃取小柱净化,利用气相色谱-质谱法,以选择离子监测模式检测,外标法进行定量分析。采用基质匹配标准溶液校准法,8种除草剂在0.010-1.000μg/L范围内线性良好,R2均大于0.990;方法检出限以信噪比≥3估算,检出限分别为:氟乐灵0.022μg/L、西玛津0.031μg/L、莠去津0.028μg/L、乙草胺0.038μg/L、甲草胺0.041μg/L、扑草净0.035μg/L、二甲戊灵0.025μg/L、丁草胺0.020μg/L。选择0.05、0.5和2.0μg/L 3个不同浓度水平做加标回收,平均回收率为74.7%-97.7%,相对标准偏差在12.0%以内。方法检出限分别为:氟乐灵0.022μg/L、西玛津0.031μg/L、莠去津0.028μg/L、乙草胺0.038μg/L、甲草胺0.041μg/L、扑草净0.035μg/L、二甲戊灵0.025μg/L、丁草胺0.020μg/L,最低定量限均为0.05μg/L。该方法具有操作简便、准确性好、灵敏度高、重现性好等优点,可为渔业水质中这8种除草剂残留的监测提供技术支持。
To measure herbicides residues in fishery water,gas chromatography-mass spectrometry was developed to determine trifluralin,pendimethalin,alachlor,acetochlor,butachlor,simazine,atrazine,and prometryn.The samples were adjusted to salinity 20-30 with Na Cl,extracted by dichloromethane,and cleaned up with Florisil solid phase extraction(SPE) column.The analytes were detected by gas chromatography-mass spectrometry under the selected reaction monitoring mode and quantified by external standard method.The peak area was linear to the concentration of eight herbicides residues(0.010-1.000 μg/L),and the correlation coefficients(R2) were all more than 0.990.According to S/N≥3,the detection limit of rifluralin,simazine,atrazine,acetochlor,alachlor,prometryn,pendimethalin,and butachlo were 0.022,0.031,0.028,0.038,0.041,0.035,0.025,and 0.020 μg/L,respectivly.The limit of quantification was 0.05 μg/L for all eight herbicides based on the actual samples spiked recoveries between 70% and 120%,S/N≥10,and the relative standard deviation≤15%.The average recovery of the eight herbicides fortified in different negative samples at 0.05,0.5,and 2.0 μg/L were in the range of 74.7%-97.7%,and the relative standard deviations were less than 12.00%.These results indicated that the method has the advantage of simplicity,sensitivity and repeatability,which could provide technical support for the detection of these eight herbicides residues in fishery water.
出处
《渔业科学进展》
CSCD
北大核心
2015年第4期132-138,共7页
Progress in Fishery Sciences
基金
福建省省属公益类科研院所基本科研专项(2012R1101-5)资助
关键词
除草剂
渔业水质
气相色谱-质谱法
检测
Herbicides
Fishery water
Gas chromatography-mass spectrometry
Detection