固相萃取−超高效液相色谱−三重四极杆质谱法同时测定海水中8种新烟碱类农药的残留

Simultaneous determination of 8 neonicotinoids pesticides in seawater by solid phase extraction-ultra performance liquid chromatography-triple quadrupole mass spectrometry

  • 摘要: 本文建立了海水中8种新烟碱类农药的固相萃取−超高效液相色谱−三重四极杆质谱(Ultra performance liquid chromatography-triple quadrupole mass spectrometry,UPLC-MS/MS)测定方法。样品经固相萃取小柱富集、净化、浓缩后,采用电喷雾离子源(electro-spray ionization,ESI)、正离子多反应监测(multiple reaction monitoring,MRM)模式进行分析,内标法定量。结果表明:8种新烟碱类农药在100 ~5000 ng/L范围内线性良好(r2>0.9990),方法检出限为0.08 ~0.14 ng/L,测定下限为0.32~0.56 ng/L。低、中、高3个水平的加标回收率分别为81.5%~98.5%、83.7%~96.8%和83.1%~96.9%,相对标准偏差分别为3.0%~7.8%、2.1%~8.8%和2.6%~8.7%。利用本方法对近岸海域12个海水样品进行检测,共检出5种不同浓度的新烟碱类农药,浓度范围为nd~82.1 ng/L,且检出的各目标化合物的MRM通道均没有明显干扰。该方法具有检出限低、灵敏度高、准确度好等优点,可以满足海水中新烟碱类农药痕量检测的要求。

     

    Abstract: A method was developed for the determination of 8 neonicotinoids in seawater by automatic solid phase extraction, ultra performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-MS/MS). After the samples were enriched, purified and concentrated by solid phase extraction (SPE), the samples were analyzed by ESI and multiple reaction selective ion monitoring (MRM) mode, and quantified by internal standard method. The results showed that 8 neonicotinoids had a good linear relationship in the range of 100−5000 ng/L (r2 > 0.9990), the detection limit of the method was between 0.08−0.14 ng/L, and the determination limit was between 0.32−0.56 ng/L. The recoveries of low, middle and high levels were 81.5%−98.5%, 83.7%−96.8% and 83.1%−96.9%, respectively, and the relative standard deviations were 3.0%−7.8%、2.1%−8.8% and 2.6%−8.7%, respectively. The method was used to detect 12 seawater samples in coastal waters, and a total of 5 neonicotinoids with different concentration ranges were detected, the concentration range was nd−82.1 ng/L, and there was no obvious interference in MRM channels of each substance detected. The method has the characteristics of low detection limit, good sensitivity and high accuracy, and is suitable for the detection of neonicotinoid pesticides in seawater.

     

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