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双固相萃取柱净化-超快速液相色谱-串联质谱法同时测定贝类组织中全氟羧酸及其前体物质

发布时间:2019-06-26 23:19
【摘要】:建立同时测定贝类中13种全氟羧酸类化合物、6种氟调聚饱和酸和3种氟调聚不饱和酸的超快速液相色谱-串联质谱分析方法。样品经90%乙腈溶液超声提取,Oasis WAX和Envi-Carb双固相萃取柱净化,Kinetex XB-C_(18)色谱柱(2.1 mm×100 mm,2.6μm)分离,多反应监测负离子模式扫描,同位素内标法定量。22种目标物在各自相应质量浓度范围内线性良好,相关系数不低于0.995,定量限为0.03~1.67 ng/g。基质加标回收率在63.05%~127.18%之间,相对标准偏差为4.70%~17.1%。本方法实现了复杂贝类基质(肌肉、肝脏、外套膜、鳃、性腺等)中PFCAs及其前体物质的同时测定,采用双柱净化方式,大大降低了杂质成分的干扰,部分化合物的灵敏度优于现有方法,适用于贝类样品中PFCAs及其前体物质的监控分析,为研究PFCAs前体物质的生物转化提供了新技术手段。
[Abstract]:A rapid liquid chromatography-tandem mass spectrometry (HPLC-MS) method for the simultaneous determination of 13 perfluorocarboxylic acids, 6 fluoropolymeric saturated acids and 3 fluoropolysaturated acids in shellfish was established. The samples were purified by ultrasonic extraction of, Oasis WAX and Envi-Carb with 90% acetonitrile solution, separated on Kinetex XB-C_ (18) column (2.1 mm 脳 100 mm, 2.6 渭 m), scanned by negative ion mode by multi-reaction monitoring, and quantified by isotope internal standard method. The 22 targets were linear in the corresponding mass concentration range, the correlation coefficient was not less than 0.99 5, and the quantitative limit was 0.03 鈮,

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