固相萃取-同位素稀释-超高效液相色谱-串联质谱法测定水中 涕灭威、涕灭威亚砜和涕灭威砜. (Chinese)

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  • Author(s): 孙慧婧; 崔冬妮
  • Source:
    Chinese Journal of Applied Chemistry; Mar2022, Vol. 39 Issue 3, p470-479, 10p
  • Additional Information
    • Alternate Title:
      Determination of Aldicarb, Aldicarb Sulfoxide, Aldicarb Sulfone in Water by Solid Phase Extraction and UPLC-MS/MS with Isotope Dilution. (English)
    • Abstract:
      A method for analysis of aldicarb, aldicarb sulfoxide and aldicarb sulfone in water was developed using solid phase extraction and HPLC-MS/MS with isotope dilution. The aqueous samples were spiked with isotope-labeled internal standards aldicarb-D3, aldicarb sulfoxide-D3 and aldicarb sulfone-D3, concentrated and purified on an HLB cartridge, and then separated on a Waters ACQUITY UPLCTM BEH C18 column by gradient elution with 0. 1% formic acid-5 mmol/L ammonium acetate-acetonitrile as the mobile phase. The analytes were detected by positive electrospray ionization with multiple reaction monitoring （MRM）. The internal standard method was used to determine the results. There is a good linearity for target compounds in the range of 0. 5~200 μg/L with the correlation coefficient（r）larger than 0. 999. The method detection limit （MDL）is 0. 0008~0. 001 μg/L. The average recoveries range between 94. 5%~105% at three different spiked levels. The relative standard deviation （RSD） is between 2. 7%~6. 5%. The method is sensitive and accurate, and is suitable for determination of aldicarb, aldicarb sulfoxide, aldicarb sulfone in water. [ABSTRACT FROM AUTHOR]
    • Abstract:
      采用同位素稀释结合固相萃取对水样进行预处理，建立了环境水体中涕灭威及其代谢物（涕灭威亚 砜、涕灭威砜）的超高效液相色谱-串联质谱分析方法。水样加同位素内标涕灭威-D3、涕灭威亚砜-D3 和涕灭威 砜-D3，经 HLB 固相萃取柱富集净化后，用 Waters ACQUITYTM BEH C18 色谱柱（2. 1 mm×100 mm，1. 7 μm）分离， 以 0. 1% 甲酸+5 mmol/L 乙酸铵水溶液-乙腈为流动相，在电喷雾离子源正离子模式下进行多反应监测（MRM）， 内标法定量。3 种目标化合物在 0. 5~200 μg/L 范围内线性良好，线性相关系数 r≥0. 999；方法检出限为 0. 0008~0. 001 μg/L，3 个加标浓度水平的平均回收率为 94. 5%~108%，相对标准偏差为 2. 7%~6. 5%。该方法 采用了稳定同位素内标参与前处理的方法，消除了涕灭威降解对测定结果的影响，准确度好、灵敏度高，可用 于环境水体中涕灭威及其代谢物涕灭威亚砜、涕灭威砜的测定。 [ABSTRACT FROM AUTHOR]
    • Abstract:
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