Benijts Tom, Günther Wolfgang, Lambert Willy, De Leenheer André
Laboratorium voor Toxicologie, Universiteit Gent, Harelbekestraat 72, B-9000 Gent, Belgium.
Rapid Commun Mass Spectrom. 2003;17(16):1866-72. doi: 10.1002/rcm.1131.
A sonic spray ionization liquid chromatography/mass spectrometry (LC/SSI-MS) procedure combined with off-line solid-phase extraction was optimized for the analysis of 20 endocrine-disrupting chemicals (EDCs) in water samples. Method development included a comparison of the novel sonic spray ionization (SSI) with more traditional ion sources, i.e. pneumatically assisted electrospray ionization (ESI) and atmospheric pressure chemical ionization (APCI). It was demonstrated that SSI and ESI spectra were very similar, but were more prone to the formation of solvent cluster ions as compared with APCI spectra. This phenomenon was most prominent for SSI and resulted in an increased chemical background in full-scan mass spectra. However, this chemical noise did not affect the overall sensitivity of SSI and ESI. After optimization of LC and MS parameters, the LC/SSI-MS method was validated. Recoveries ranged from 76.3 up to 113.4% for all compounds. Limits of detection (LOD) and quantitation (LOQ) were established between 3.0 and 11.5 ng/L and 9.9 and 38.0 ng/L, respectively. Within-day (n = 5) and between-day (n = 5) reproducibility were investigated at three levels and ranged from 3.3-16.5% and 7.6-19.2%, respectively. Eight-point calibration curves were established and showed linearity for all compounds (r(2) > 0.987) over a linear dynamic range of 10-10 000 ng/L.
一种结合离线固相萃取的超声喷雾电离液相色谱/质谱(LC/SSI-MS)方法被优化用于分析水样中的20种内分泌干扰化学物质(EDC)。方法开发包括将新型超声喷雾电离(SSI)与更传统的离子源进行比较,即气动辅助电喷雾电离(ESI)和大气压化学电离(APCI)。结果表明,SSI和ESI光谱非常相似,但与APCI光谱相比,更容易形成溶剂簇离子。这种现象在SSI中最为突出,导致全扫描质谱中的化学背景增加。然而,这种化学噪声并不影响SSI和ESI的整体灵敏度。在优化LC和MS参数后,对LC/SSI-MS方法进行了验证。所有化合物的回收率在76.3%至113.4%之间。检测限(LOD)和定量限(LOQ)分别在3.0至11.5 ng/L和9.9至38.0 ng/L之间。在三个水平上研究了日内(n = 5)和日间(n = 5)的重现性,分别为3.3 - 16.5%和7.6 - 19.2%。建立了八点校准曲线,所有化合物在10 - 10000 ng/L的线性动态范围内均显示出线性(r(2) > 0.987)。