University of Lisbon, Faculty of Sciences, Chemistry and Biochemistry Department, Campo Grande Ed. C8, 1749-016, Lisbon, Portugal.
Anal Bioanal Chem. 2010 Mar;396(5):1853-62. doi: 10.1007/s00216-009-3392-6. Epub 2010 Jan 5.
Stir-bar-sorptive extraction with liquid desorption followed by large-volume injection and capillary gas chromatography coupled to mass spectrometry in selected ion monitoring acquisition mode (SBSE-LD/LVI-GC-MS(SIM)) has been developed to monitor ultra-traces of four musks (celestolide (ADBI), galaxolide (HHCB), tonalide (AHTN) and musk ketone (MK)) in environmental water matrices. Instrumental calibration (LVI-GC-MS(SIM)) and experimental conditions that could affect the SBSE-LD efficiency are discussed. Assays performed on 30-mL water samples spiked at 200 ng L(-1) under optimized experimental conditions yielded recoveries ranging from 83.7 ± 8.1% (MK) to 107.6 ± 10.8% (HHCB). Furthermore, the experimental data were in very good agreement with predicted theoretical equilibria described by octanol-water partition coefficients (K (PDMS/W) ≈ K (O/W)). The methodology also showed excellent linear dynamic ranges for the four musks studied, with correlation coefficients higher than 0.9961, limits of detection and quantification between 12 and 19 ng L(-1) and between 41 and 62 ng L(-1), respectively, and suitable precision (< 20%). Application of this method for analysis of the musks in real water matrices such as tap, river, sea, and urban wastewater samples resulted in convenient selectivity, high sensitivity and accuracy using the standard addition methodology. The proposed method (SBSE-LD/LVI-GC-MS(SIM)) was shown to be feasible and sensitive, with a low-sample volume requirement, for determination of musk compounds in environmental water matrices at the ultra-trace level, overcoming several disadvantages presented by other sample-preparation techniques.
搅拌棒吸附萃取结合液液解吸和大体积进样-毛细管气相色谱-质谱联用选择离子监测模式（SBSE-LD/LVI-GC-MS(SIM)）已被开发用于监测环境水样中四种麝香（天来麝香（ADBI）、加洛麝香（HHCB）、泰勒麝香（AHTN）和酮麝香（MK））的痕量。讨论了仪器校准（LVI-GC-MS(SIM))和可能影响 SBSE-LD 效率的实验条件。在优化的实验条件下，对 30 毫升加标 200 ng/L 的水样进行测定，MK 的回收率为 83.7 ± 8.1%，HHCB 的回收率为 107.6 ± 10.8%。此外，实验数据与辛醇-水分配系数（K(PDMS/W)≈K(O/W)）描述的理论平衡非常吻合。该方法还表现出对所研究的四种麝香极好的线性动态范围，相关系数均高于 0.9961，检测限和定量限分别为 12-19 ng/L 和 41-62 ng/L，精密度良好（<20%）。应用该方法对自来水、河水、海水和城市污水等实际水样中的麝香进行分析，结果表明，该方法选择性好、灵敏度高、准确度高，采用标准添加法。该方法（SBSE-LD/LVI-GC-MS(SIM)）具有灵敏度高、所需样品体积小的优点，适用于环境水样中痕量麝香化合物的测定，克服了其他样品前处理技术的一些缺点。
