Department of Analytical Chemistry, University of the Basque Country, P. K. 644, 48080 Bilbao, Spain; Laboratoire de Chimie Analytique Bio-inorganique et Environnement, Institut Pluridisciplinaire de Recherche sur l'Environnement et les Matériaux, CNRS UMR 5254, Université de Pau et des Pays de l'Adour, Hélioparc Pau Pyrénées, 2, av. P. Angot, 64053 Pau cedex 9, France.
Department of Analytical Chemistry, University of the Basque Country, P. K. 644, 48080 Bilbao, Spain; IKERBASQUE, Basque Foundation for Science, 48011 Bilbao, Spain; Department of Analytical Chemistry, Helmholtz Centre for Environmental Research-UFZ Permoserstraße 15, D-04318 Leipzig, Germany.
Anal Chim Acta. 2013 Apr 22;773:68-75. doi: 10.1016/j.aca.2013.02.036. Epub 2013 Mar 1.
In this work the development and validation of a new procedure for the simultaneous determination of 9 nitro and polycyclic musk compounds: musk ambrette (MA), musk ketone (MK), musk mosken (MM), celestolide (ADBI), phantolide (AHMI), tonalide (AHTN), traseolide (ATII), cashmeran (DPMI) and galaxolide (HHCB) in environmental water samples (estuarine and wastewater) using microextraction by packed sorbent (MEPS) followed by large volume injection-gas chromatography-mass spectrometry (LVI-GC-MS) was carried out. Apart from the optimization of the different variables affecting MEPS (i.e., nature of the sorbent, nature of the solvent elution, sample load, and elution/injection volume) extraction recovery was also evaluated, not only for water samples but also for environmental water matrices such as estuarine and waste water. The use of two deuterated analogs ([(2)H3]-AHTN and [(2)H15]-MX) was successfully evaluated in order to correct matrix effect in complex environmental matrices such as influent samples from wastewater treatment plants. Method detection limits (MDLs) ranged from 5 to 25 ng L(-1), 7 to 39 ng L(-1) and 8 to 84 ng L(-1) for influent, effluent and estuarine samples, respectively. Apparent recoveries were higher than 75% for all target compounds in all the matrices studied (estuarine water and wastewater) and the precision of the method, calculated as relative standard deviation (RSD), was below 13.2% at 200 ng L(-1) concentration level and below 14.9% at low level (20 ng L(-1) for all the target analytes, except for AHTN which was set at 40 ng L(-1) and HHCB at 90 ng L(-1), due to the higher MDL values presented by those target compounds). Finally, this MEPS procedure was applied to the determination of the target analytes in water samples, including estuarine and wastewater, from two estuaries, Urdaibai (Spain) and Adour (France) and an established stir-bar sorptive extraction-liquid desorption/large volume injection-gas chromatography-mass spectrometry (SBSE-LD/LVI-GC-MS) method was performed in parallel for comparison. Results were in good agreement for all the analytes determined, except for DPMI.
本工作开发并验证了一种新方法，用于同时测定环境水样（河口和废水）中的 9 种硝基和多环麝香化合物：麝香甲酮（MK）、麝香酮（MA）、麝香紫（MM）、环十五内酯（ADBI）、磷氮酸二甲酯（AHMI）、六氢-1,3,5-三甲基-4,6-二硝基苯（AHTN）、吐纳麝香（ATII）、葵子麝香（DPMI）和加乐麝香（HHCB）。该方法采用微萃取填充固相（MEPS）结合大体积进样-气相色谱-质谱联用（LVI-GC-MS），在优化影响 MEPS 的不同变量的同时（即吸附剂的性质、洗脱溶剂的性质、样品负荷和洗脱/进样体积），还评估了萃取回收率，不仅针对水样，还针对河口和废水等环境水样基质。成功评估了两种氘代类似物[（2）H3]-AHTN 和[（2）H15]-MX 的使用，以校正复杂环境基质（如来自废水处理厂的进水样品）中的基质效应。对于进水、出水和河口样品，方法检测限（MDL）分别为 5 至 25ng/L、7 至 39ng/L 和 8 至 84ng/L。所有目标化合物在所有研究的基质（河口水和废水）中的表观回收率均高于 75%，方法的精密度（以相对标准偏差（RSD）表示）在 200ng/L 浓度水平下低于 13.2%，在低浓度（20ng/L）下低于 14.9%（除 AHTN 外，所有目标分析物的浓度均为 20ng/L，HHCB 的浓度为 90ng/L，因为这些目标化合物的 MDL 值较高）。最后，该 MEPS 程序应用于两个河口（西班牙的 Urdaibai 和法国的 Adour）的水样中目标分析物的测定，并与建立的搅拌棒吸附萃取-液体解吸/大体积进样-气相色谱-质谱（SBSE-LD/LVI-GC-MS）方法进行了平行比较。除 DPMI 外，所有测定的分析物结果均一致。
