Analysis of 35 priority semivolatile compounds in water by stir bar sorptive extraction-thermal desorption-gas chromatography-mass spectrometry Part II:: Method validation

被引:66
作者
León, VM [1 ]
Llorca-Pórcel, J [1 ]
Alvarez, B [1 ]
Cobollo, MA [1 ]
Muñoz, S [1 ]
Valor, I [1 ]
机构
[1] Labaqua SA, Alicante 03007, Spain
关键词
stir bar sorptive extraction; water analysis; pesticides; PAHs; method validation; GC-MS;
D O I
10.1016/j.aca.2005.10.080
中图分类号
O65 [分析化学];
学科分类号
070302 ; 081704 ;
摘要
A multiresidue method for the determination of 35 organic micropollutants, pesticides, and polycyclic aromatic hydrocarbons (PAHs) in water using stir bar sorptive extraction (SBSE) and thermal desorption coupled to capillary gas chromatography-mass spectrometry (SBSE-TD-GC-MS) has been validated. Method sensitivity, linearity, repeatability and reproducibility, accuracy, matrix effects, and overall uncertainties have been studied for method validation according to the international norm ISO/IEC 17025:1999. The quantification limits ranged from 0.1 to 36 ng/L working in the MS full scan mode. Correlation coefficients of the calibration curves from 20 to 600 ng/L were higher than 0.990 for all the compounds. To validate matrix effects for tap water, ground water and surface water, repeatability, reproducibility, accuracy and overall uncertainty were calculated for the three matrices at 50 and 500 ng/L levels. The accuracy of the method was also evaluated by participating in a proficiency interlaboratory test with real samples. (c) 2005 Elsevier B.V. All rights reserved.
引用
收藏
页码:261 / 266
页数:6
相关论文
共 16 条
[1]   SOLID-PHASE MICROEXTRACTION WITH THERMAL-DESORPTION USING FUSED-SILICA OPTICAL FIBERS [J].
ARTHUR, CL ;
PAWLISZYN, J .
ANALYTICAL CHEMISTRY, 1990, 62 (19) :2145-2148
[2]  
Baltussen E, 1999, J MICROCOLUMN SEP, V11, P737, DOI 10.1002/(SICI)1520-667X(1999)11:10<737::AID-MCS7>3.0.CO
[3]  
2-4
[4]   ENVIRONMENTAL-PROTECTION-AGENCY AND OTHER METHODS FOR THE DETERMINATION OF PRIORITY PESTICIDES AND THEIR TRANSFORMATION PRODUCTS IN WATER [J].
BARCELO, D .
JOURNAL OF CHROMATOGRAPHY, 1993, 643 (1-2) :117-143
[5]   Strategies for the extraction of free and bound polycyclic aromatic hydrocarbons in run-off waters rich in organic matter [J].
García-Falcón, MS ;
Pérez-Lamela, C ;
Simal-Gándara, J .
ANALYTICA CHIMICA ACTA, 2004, 508 (02) :177-183
[6]   Stirring bar sorptive extraction in the determination of PAHs in drinking waters [J].
García-Falcón, MS ;
Cancho-Grande, B ;
Simal-Gándara, J .
WATER RESEARCH, 2004, 38 (07) :1679-1684
[7]   Trace analysis of phenolic xenoestrogens in water samples by stir bar sorptive extraction with in situ derivatization and thermal desorption-gas chromatography-mass spectrometry [J].
Kawaguchi, M ;
Inoue, K ;
Yoshimura, M ;
Sakui, N ;
Okanouchi, N ;
Ito, R ;
Yoshimura, Y ;
Nakazawa, H .
JOURNAL OF CHROMATOGRAPHY A, 2004, 1041 (1-2) :19-26
[8]   Determination of 4-nonylphenol and 4-tert-octylphenol in water samples by stir bar sorptive extraction and thermal desorption gas chromatography mass spectrometry [J].
Kawaguchi, M ;
Inoue, K ;
Yoshimura, M ;
Ito, R ;
Sakui, N ;
Nakazawa, H .
ANALYTICA CHIMICA ACTA, 2004, 505 (02) :217-222
[9]   Application of stir bar sorptive extraction to the determination of polycyclic aromatic hydrocarbons in aqueous samples [J].
Kolahgar, B ;
Hoffmann, A ;
Heiden, AC .
JOURNAL OF CHROMATOGRAPHY A, 2002, 963 (1-2) :225-230
[10]   Analysis of 35 priority semivolatile compounds in water by stir bar sorptive extraction-thermal desorption-gas chromatography-mass spectrometry I.: Method optimisation [J].
León, VM ;
Alvarez, B ;
Cobollo, MA ;
Muñoz, S ;
Valor, I .
JOURNAL OF CHROMATOGRAPHY A, 2003, 999 (1-2) :91-101