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固相萃取净化-超高效液相色谱串联质谱测定水产品中氯硝柳胺 被引量:2

Determination of Niclosamide in Aquatic Products Based on Solid Phase Extraction Coupled with Liquid Chromatography Tandem Mass Spectrometry
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摘要 建立了水产品中氯硝柳胺的固相萃取净化-液相色谱串联质谱分析方法。样品经2%氨水乙腈溶液提取,弗罗里硅土柱净化,液相色谱串联质谱分析。在ACQUITY UPLC BEH C18色谱柱上进行分离,采用梯度洗脱,电喷雾正离子电离,多反应监测模式,外标法定量。结果表明,氯硝柳胺在2.5-100μg/L浓度范围内线性相关系数均大于0.999,对应的检出限和定量限均为0.2μg/kg和0.5μg/kg,平均回收率为86.8%-91.3%;相对标准偏差为3.14%-6.74%。本方法基质干扰小、净化效果强、灵敏度高,适合水产品中氯硝柳胺的分析测定。 A new method of solid phase extraction combined with high liquid chromatography-tandem mass spectrometry was established for the determination of niclosamide in aquatic products. The sample was extracted with 2%ammonia acetonitrile solution, cleaned up by florisil coupled with high performance liquid chromatography-mass spectrometry. The chromatographic separation was performed on an ACQUITY UPLC BEH C18 column with gradient elution. External standard method was used for quantification and the positive electrospray ionization source under the multiple reaction monitoring mode. Linear ranges of niclosamide was in the range of 2. 5 - 100 μg/L with correlation coefficient more than 0. 999. The limit of detection(LOD) and limit of quantification(LOQ) for niclosamide was calculated as 0. 2 and 0. 5 μg/kg. The recoveries of analyte in sample were in the range of 86. 8% - 91. 3% with the relative standard deviation of less than 6. 74%. Therefore,the method could be used to identify and quantify niclosamide in aquatic products with less matrix interference and satisfactory sensitive.
出处 《广州化工》 CAS 2016年第22期81-83,共3页 GuangZhou Chemical Industry
基金 浙江省科研院所公共科技服务项目(2016F30022)
关键词 氯硝柳胺 固相萃取 液相色谱串联质谱 niclosamide solid phase extraction high performance liquid chromatography-mass spectrometry
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