| 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0.010−1.000 µg/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0.022 µg/L、西玛津0.031 µg/L、莠去津0.028 µg/L、乙草胺0.038 µg/L、甲草胺0.041 µg/L、扑草净0.035 µg/L、二甲戊灵0.025 µg/L、丁草胺0.020 µg/L。选择0.05、0.5和2.0 µg/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0.022 µg/L、西玛津0.031 µg/L、莠去津0.028 µg/L、乙草胺0.038 µg/L、甲草胺0.041 µg/L、扑草净0.035 µg/L、二甲戊灵0.025 µg/L、丁草胺0.020 µg/L，最低定量限均为0.05 µg/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。 |
| 关键词: 除草剂 渔业水质 气相色谱-质谱法 检测 |
| DOI：10.11758/yykxjz.20150420 |
| 分类号: |
| 基金项目:福建省省属公益类科研院所基本科研专项(2012R1101-5)资助 |
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| Determination of Eight Herbicides in Fishery Water by Gas Chromatography-Mass Spectrometry |
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LUO Fangfang,,WANG Yanjun,YE Mei,YU Ying,LIU Haixin,JIANG Linlin
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Fisheries Research Institute of Fujian, Xiamen 361012
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| Abstract: |
| 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 NaCl, 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. |
| Key words: Herbicides Fishery water Gas chromatography-mass spectrometry Detection |
