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快速固相萃取/超高效液相色谱-串联质谱法测定水产品中25种磺酰脲类及磺酰胺类除草剂残留
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朱富强,吴树栋,韩岩君,郭宇鹏 滨州市检验检测中心山东 滨州 256600 
中文摘要:建立了快速固相萃取结合超高效液相色谱-串联质谱(UPLC-MS/MS)同时测定水产品中25种磺酰脲类及磺酰胺类除草剂残留的分析方法。样品以乙腈提取、盐析除水后,经SHIMSEN QVet-NM + 固相萃取柱净化,采用Shim-pack GIST C18柱(2.1 mm × 50 mm × 2.0 μm)进行液相色谱分离,以0.1%甲酸水溶液-乙腈作为流动相进行梯度洗脱。采用电喷雾电离源、多反应监测(MRM)模式进行定量分析,以基质匹配标准溶液外标法定量。结果表明,25种待测化合物在0.20 ~ 50 μg/L范围内线性关系良好(r2 > 0.994),方法检出限(LOD)为0.30 ~ 1.3 μg/kg,定量下限(LOQ)为1.2 ~ 5.0 μg/kg,在3个加标水平的回收率为62.7% ~ 122%,相对标准偏差(RSD)为0.72% ~ 18%。该方法简便快速,准确性好、灵敏度高,可为水产品中农药残留的监控提供一种更为高效的技术支持。
中文关键词:磺酰脲类  磺酰胺类  水产品  超高效液相色谱-串联质谱法  快速固相萃取
 
Determination of 25 Sulfonylurea Herbicides and Triazolopyrimidine Sulfonamides Herbi?cides in Aquatic Products by Ultra Perfor?mance Liquid Chromatography-Tandem Mass Spectrometry with Rapid Solid Phase Extraction
Abstract:A rapid and accurate analysis method based on rapid solid phase extraction and ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) was developed for the determination of 25 kinds of sulfonylurea herbicides and triazolopyrimidine sulfonamides herbicides in aquatic products. Firstly, the pretreatment conditions for the 25 pesticides in aquatic product samples were systematically optimized, based on recoveries, purification efficiencies and other factors, acetonitrile was used as the extraction solvent, and a SHIMSEN QVet-NM + rapid solid phase extraction cartridge was selected as the pretreatment purification column. Then, the chromatographic conditions and MS parameters were optimized. Finally, the chromatographic separation was performed on a Shim-pack GIST C18(2.1 mm × 50 mm × 2.0 μm) column under linear gradient elution using 0.1% formic acid solution and acetonitrile as the mobile phases. The 25 kinds of sulfonylurea herbicides and triazolopyrimidine sulfonamides herbicides were detected by triple quadrupole MS with electrospray ionization(ESI) in multiple reaction monitoring(MRM) mode under both positive and negative conditions, and quantified by a matrix-matched external standard method. The 25 herbicides showed good linear relationships in the concentration range of 0.20-50 μg/L with correlation coefficients(r2) greater than 0.994. The limits of detection(LOD) and limits of quantitation(LOQ) were in the ranges of 0.30-1.3 μg/kg and 1.2-5.0 μg/kg, respectively. The average recoveries for the analytes at three spiked levels varied from 62.7% to 122%, with the relative standard deviations(RSD) of 0.72%-18%. Results of the matrix effects(ME) for 25 herbicides showed that all of the herbicides exhibited matrix inhibition effects in grass carp, penaeus vannamei and meretrix meretrix. The matrix effects could be reduced by the matrix-matched standard curve method. The method was applied to the detection of 25 herbicides in aquatic product samples. None of them were found in the samples. The experimental results indicated that the proposed method was simple, quick, accurate and sensitive, and was suitable for the determination of 25 kinds of sulfonylurea herbicides and triazolopyrimidine sulfonamides herbicides in aquatic products.
Key Words:sulfonylurea herbicides  triazolopyrimidine sulfonamides herbicides  aquatic products  ultra performance liquid chromatography-tandem mass spectrometry  rapid solid phase extraction
引用本文:朱富强,吴树栋,韩岩君,郭宇鹏.快速固相萃取/超高效液相色谱-串联质谱法测定水产品中25种磺酰脲类及磺酰胺类除草剂残留[J].分析测试学报,2021,40(9):1279-1285.
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