| 加速溶剂萃取/液相色谱-串联质谱测定底泥中氯硝柳胺及其降解产物 |
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| 基金项目:江西省现代农业科研协同创新专项（JXXTCX201602-06）；国家畜禽产品风险评估专项（GJFP2017007） |
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| 中文摘要:建立了加速溶剂萃取/液相色谱-串联质谱分析底泥中氯硝柳胺及其降解产物（5 氯水杨酸和2 氯 4 硝基苯胺）的方法。以中性氧化铝作为池内吸附材料，集提取和净化于一步，乙腈-水（3∶1，体积比）作为萃取溶剂，优化了温度和静态萃取时间等参数。在优化条件下，氯硝及其降解产物在01~200 μg/L范围内有良好线性关系，相关系数（r）均大于0999。方法的检出限和定量下限分别为004~01 μg/kg和02~05 μg/kg。用于底泥中氯硝柳胺及其降解产物的分析，在05、10、20 μg/kg加标水平下，平均加标回收率为 935%~1019%，相对标准偏差为37%~67%。该方法简便，灵敏度高，重现性好，可应用于实际样品分析。 |
| 中文关键词:液相色谱-串联质谱法（LC-MS/MS） 氯硝柳胺 降解产物 加速溶剂萃取 底泥 |
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| Determination of Niclosamide and Its Degradation Products in Sediments with Accelerated Solvent Extraction/Liquid Chromatography-Tandem Mass Spectrometry |
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| Abstract:A method based on liquid chromatography-tandem mass spectrometry with accelerated solvent extraction（ASE/LC-MS/MS） was developed for the analysis of niclosamide and its degradation products（5 chlorosalicylic acid and 2 chloro 4 nitroaniline） in sediments.Extraction and cleanup were integrated into one step by accelerated solvent extraction（ASE） with 50 g neutral alumina as within cell adsorbing material,and different temperatures and static times were optimized with acetonitrile-water（3∶1,by volume） as extraction solvents.Under the optimized conditions,the calibration curves for niclosamide and its degradation products were linear in the range of 01-200 μg/L with their correlation coefficients（r） more than 0999.The limits of detection and quantitation of the method were in the ranges of 004-01 μg/kg and 02-05 μg/kg,respectively.The proposed method was applied in the trace analysis of niclosamide and its degradation products in sediments with average recoveries in the range of 935%-1019% at 3 spiked levels of 05,10 and 20 μg/kg,and relative standard deviations of 37%-67%.The method was simple,sensitive and reproducible,and was suitable for the analysis of real sample. |
| Key Words:liquid chromatography tandem mass spectrometry（LC-MS/MS） niclosamide degradation products accelerated solvent extraction sediment |
| 引用本文：廖且根，张大文，罗林广.加速溶剂萃取/液相色谱-串联质谱测定底泥中氯硝柳胺及其降解产物[J].分析测试学报,2018,37(7):825-829. |
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