高级检索

    QuEChERS-高效液相色谱-串联质谱法同时测定生活饮用水中11种新烟碱类杀虫剂的含量

    Simultaneous Determination of 11 Neonicotinoid Pesticides in Domestic Drinking Water by HPLC-MS/MS with QuEChERS

    • 摘要: 提出了QuEChERS-高效液相色谱-串联质谱法(HPLC-MS/MS)同时测定生活饮用水中11种新烟碱类杀虫剂(吡虫啉、烯啶虫胺、啶虫脒、噻虫啉、氯噻啉、环氧虫啶、噻虫嗪、噻虫胺、呋虫胺、氟啶虫胺腈、氟啶虫酰胺)含量的方法。5 mL过滤后的水样用含1%(体积分数)甲酸的二氯甲烷溶液提取两次,合并下层提取液,氮吹至干,加入50 mg N-丙基乙二胺(PSA)和1 mL体积比65∶35的0.2%(体积分数,下同)甲酸溶液-乙腈的混合溶液,涡旋后过0.22 μm聚醚砜滤膜。以不同体积比的0.2%甲酸溶液-乙腈的混合溶液为流动相进行梯度洗脱,分离后的11种目标物经电喷雾离子源正离子模式扫描,以多反应监测模式检测,外标法定量。结果表明:11种新烟碱类杀虫剂的质量浓度在一定范围内与对应的峰面积呈线性关系,测定下限(10S/N)为0.02~0.08 μg·L-1;在3个加标浓度水平下,11种目标物的回收率为62.1%~101%,测定值的相对标准偏差(n=6)为5.0%~15%。方法用于8份自来水、4份河水和3份水库水样品分析,结果显示4份河水样品和2份水库水样品中检出新烟碱类杀虫剂(噻虫胺、吡虫啉、噻虫嗪、啶虫脒),其余样品中均为检出目标物。

       

      Abstract: A method for the simultaneous determination 11 neonicotionid pesticides, including imidacloprid, nitenpyram, acetamiprid, thiacloprid, imidaclothiz, cycloxaprid, thiamethoxam, clothianidin, dinotefuran, sulfoxaflor and flonicamid in domestic drinking water by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) with QuEChERS was proposed. The filtered water sample (5 mL) was extracted twice with dichloromethane solution containing 1% (volume fraction) formic acid. Then the lower extract solutions were combined and blown to dryness by nitrogen, and 50 mg of N-propyl ethylenediamine (PSA) and 1 mL of the mixed solution composed of 0.2% (volume fraction, the same below) formic acid solution and acetonitrile at volume ratio of 65\:35 were added. After vortex, the above solution was passed through 0.22 μm polyether sulfone filter membrane. The mixed solutions composed of 0.2% formic acid solution and acetonitrile at different volume ratios were used as the mobile phase for gradient elution. The separated 11 targets were scanned by electrospray ion source with positive ion mode, detected by multiple reaction monitoring mode, and quantified by external standard method. As shown by the results, linear relationships between the mass concentrations and corresponding peak areas of 11 neonicotionid pesticides were kept in definite ranges, with lower limits of determination (10S/N) in the range of 0.02-0.08 μg·L-1. The recoveries of 11 targets were in the range of 62.1%-101% at 3 spiked concentration levels, and RSDs (n=6) of the determined values ranged from 5.0% to 15%. The method was applied to analysis of 8 samples of tap water, 4 samples of river water and 3 samples of reservoir water. It was shown that neonicotionid pesticides including clothianidin, imidacloprid, thiamethoxam and acetamidine were deteceted in 4 samples of river water and 2 samples of reservoir water, and the other samples were not detected targets.

       

    /

    返回文章
    返回