环境水样与生物组织中六溴环十二烷异构体分析新方法研究-环境科学专业论文.docxVIP

山东建筑大学硕士学位论文 (GCB)、120mg中性氧化铝、100mg无水硫酸镁、2．5mL乙腈和lmL血液样 品。在最优条件下空白样品基质加标回收率为83．6。115．0％，相对标准偏差@SD) 为o．5．9．5％，方法检测限为0．04．0．19 ng／mL。在两个实际鸡全血液样品中分别检 出有士泓船CD和卸．HBCD，且其EF值(手性异构对映体分数)大于O．5。以上 数据说明，该方法可满足检测血液中低浓度的HBCDs的要求。将QuEChERS法 应用与血液中HBCDs的检测，结果表明所建立的方法具有简单、高效、成本低、 精密度高、检测限低等特点，适用于实际样品的常规批量分析。 (3)建立了基于基质固相分散同位素稀释联合液相色谱串联质谱联用技术 (MSPD．ISD．LC-MS／MS)对鸡肉中HBCD三种异构体及其手性异构的快速分 析方法。以单因素优化实验确定最佳分散剂为弗罗里硅土、乙腈取得最高萃取 效率，通过正交试验得出最佳用量为：o．59鸡肉、1．29十八烷基硅胶(C18)、 lg弗罗里硅土和5mL乙腈。在最优条件下空白样品基质加标回收率为 84．0．117．3％，相对标准偏差为4．6．12．5％，方法检测限为O．05．0．18ng／g。以上数 据表明，该方法可满足检测鸡肉中痕量HBCDs的要求。同时将同位素稀释法应 用于LC．MS—MS分析技术中消除了基质效应的影响。实验结果表明该方法简单、 高效、精密度高，具有十分重要的实际应用价值。 关键词：六溴环十二烷，室温离子液体，QuEChERS，基质固相分散，液相 色谱串联质谱 万方数据  山东建筑大学硕士学位论文 A new determination of Hexabromocyclododecane enantiomers ● ● ● ■ ’ ●’ ● - ● l ·‘ in envlmnmental water samples and biOlogical ussUeS Yao Yuxiang(Environmental Engineering) Directed by Sun Youmin ABSTRACT In this paper,the nature，the source of the pollution situation and enrichment， purification and analysis method of HBCD(Hexabromocylcododecane，HBCDs) were reviewed comprehensively．So far there is no universal method of analysis in domestic and foreign．This study develops the sample determination techniques systematically and the factors influencing recovery and sensitivity were investigated and optimized with single factor experiment and orthogonal experiment． Ultrasound．assisted ionic liquid dispersive liquid liquid microextraction (USA-IL．DLLME)coupled with liquid chromatography and tandem quadmpole mass spectrometry(LC．MS／MS)was developed for determination of HBCDs in environmental water samples；QuEChERs approach followed by liquid chromatography coupled with tandem mass spectrometry(LC·ESI·MS／MS)method has been developed for the determination of hexabromocyclododecane enantiomers (土％邙and+7-HBCD)in chicken blood；MSPD procedure has been developed for the determination of hexabromocyclododecane enantiomers(土a，邙and士-T-I-IBCD) in chicken muscl