固相萃取-超高效液相色谱-串联质谱法测定海水中13种三嗪类除草剂残留量

任传博; 田秀慧; 张华威; 刘云; 孙岩; 徐英江; 宫向红; 王茂剑

doi:10.7538/zpxb.2013.34.06.0353

固相萃取-超高效液相色谱-串联质谱法测定海水中13种三嗪类除草剂残留量

任传博^1,2,
田秀慧^1,3,
张华威^1,2,
刘云⁴,
孙岩^1,3,
徐英江^1,3,
宫向红^1,3,
王茂剑^1,3

1.
山东省海洋水产研究所, 山东烟台264006
2.
烟台山水海产有限公司, 山东烟台264006
3.
山东省海洋生态修复重点实验室, 山东烟台264006
4.
上海海洋大学食品学院, 上海201306

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- 刊出日期: 2013-11-19

Determination of Triazine Herbicides in Seawater Using Solid Phase Extraction-UPLC-MS/MS

1.
Marine Fisheries Research Institute of Shandong Province, Yantai 264006, China
2.
Yantai Shanshui Seafood Co. Ltd, Yantai 264006, China
3.
Shandong Province Key Laboratory of Restoration for Marine Ecology, Yantai 264006, China
4.
College of Food Science and Technology, Shanghai Ocean University, Shanghai 201306, China

摘要

摘要: 建立了固相萃取超高效液相色谱串联质谱法测定海水中13种三嗪类除草剂，样品抽滤后，经HLB固相萃取柱浓缩净化，洗脱液40 ℃下氮气吹至小于1 mL，然后用V（乙腈）∶V（水）=1∶1的溶液定容至1 mL，超声振荡1 min，样液经0.22 μm滤膜，在Acquity^TM UPLC HSS C18（2.1 mm ×100 mm×1.8 μm）色谱柱上进行梯度洗脱分离。流动相为乙腈和含有0.1%甲酸的5 mmol/L乙酸铵溶液，多反应监测模式下测定13种三嗪类除草剂残留量。13种三嗪类除草剂的线性范围为1~50 ng/L，相关系数为0.992~0.999；检出限为1 ng/L，定量限为2 ng/L，在2、5、10 ng/L 3个浓度水平加标平均回收率为65.8%~103%，相对标准偏差RSD为4.84%~15.2%。该方法灵敏度高、准确性好，适用于海水中除草剂类药物的检测。
- 三嗪类 /
- 海水 /
- 超高效液相色谱-串联质谱 /
- 固相萃取
Abstract: The triazine herbicides in seawater were determined by solid phase extraction ultra performance liquid chromatography with electrospray ionization tandem mass spectrometry(UPLC-ESI-MS/MS). UPLC and MS/MS analytical conditions were examined and optimized critically by a series of experiments. Samples were filtrated and purified on the HLB solid phase extraction cartridges. The elution was collected and evaporated to less than 1 mL at 40 ℃ by nitrogen blow, then added to 1 mL acetonitrile and water (1∶1，V/V) and ultrasonic wave extraction for 1 min. After filtrated with 0.22 μm filter membrane, the residue was separated by Acquity^TMUPLC HSS C18 column (2.1 mm×100 mm×1.8 μm) using gradient elution separation. The mobile phase was a mixture of A (acetonitrile) and B (5 mmol/L ammonium acetate containing 0.1% formic acid) in a flow rate of 0.25 mL/min. Finally analytes were confirmed and quantified using MS/MS system in multiple reaction mode with triple quadrapole analyzer using positive polarity mode. The analytes show good linearity in the range of 1 ng/L to 50 ng/L with correlation coefficient from 0.992 to 0.999. The detection limit is 1 ng/L，and quantification limit is 2 ng/L. The average recoveries at three dose levels(2 ng/L, 5 ng/L and 10 ng/L) are 65.8%—103% with relative standard deviations from 4.84% to 15.2%. In addition, the method has merits of simplicity, sensitivity and rapidity, and can be used for simultaneous determination of triazine herbicides in seawater.
- triazine /
- seawater /
- ultra performance liquid chromatography tandem mass spectrometry /
- solid phase extraction

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参考文献(21)

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固相萃取-超高效液相色谱-串联质谱法测定海水中13种三嗪类除草剂残留量

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Determination of Triazine Herbicides in Seawater Using Solid Phase Extraction-UPLC-MS/MS

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