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  

Determination of Niclosamide and Its Degradation Products in Sediments with Accelerated Solvent Extraction/Liquid Chromatography-Tandem Mass Spectrometry

作　　者：廖且根[1] 张大文[1] 罗林广[1] LIAO Qie-gen;ZHANG Da-wen;LUO Lin-guang(Agricultural Product Quality Safety and Standards Institute,Jiangxi Academy of Agricultural Sciences,Nanchang 330200,Chin)

机构地区：[1]江西省农业科学院农产品质量安全与标准研究所,江西南昌330200

出　　处：《分析测试学报》2018年第7期825-829,共5页Journal of Instrumental Analysis

基　　金：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)

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0.1~20.0μg/L范围内有良好线性关系,相关系数(r)均大于0.999。方法的检出限和定量下限分别为0.04~0.1μg/kg和0.2~0.5μg/kg。用于底泥中氯硝柳胺及其降解产物的分析,在0.5、1.0、2.0μg/kg加标水平下,平均加标回收率为93.5%~101.9%,相对标准偏差为3.7%~6.7%。该方法简便,灵敏度高,重现性好,可应用于实际样品分析。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 5. 0 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 0. 1-20. 0 μg/L with their correlation coefficients（r） more than 0. 999. The limits of detection and quantitation of the method were in the ranges of 0. 04-0. 1 μg/kg and 0. 2-0. 5 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 93. 5%-101. 9% at 3 spiked levels of 0. 5,1. 0 and2. 0 μg/kg,and relative standard deviations of 3. 7%-6. 7%. The method was simple,sensitive and reproducible,and was suitable for the analysis of real sample.

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 

分 类 号：O657.63[理学—分析化学] F767.2[理学—化学]