El Aribi Houssain, Le Blanc Yves J C, Antonsen Stephen, Sakuma Takeo
Applied Biosystems/MDS Sciex, 71 Four Valley Drive, Concord, Ont., Canada L4K 4V8.
Anal Chim Acta. 2006 May 10;567(1):39-47. doi: 10.1016/j.aca.2006.03.012. Epub 2006 Apr 18.
A new IC-ESI-MS/MS method, with simple sample preparation procedure, has been developed for quantification and confirmation of perchlorate (ClO4-) anions in water, fresh and canned food, wine and beer samples at low part-per-trillion (ng l(-1)) levels. To the best of our knowledge, this is the first time an analytical method is used for determination of perchlorate in wine and beer samples. The IC-ESI-MS/MS instrumentation consisted of an ICS-2500 ion chromatography (IC) system coupled to either an API 2000 or an API 3200 mass spectrometer. The IC-ESI-MS/MS system was optimized to monitor two pairs of precursor and fragment ion transitions, i.e., multiple reaction monitoring (MRM). All samples had oxygen-18 isotope labeled perchlorate internal standard (ISTD) added prior to extraction. Chlorine isotope ratio (35Cl/37Cl) was used as a confirmation tool. The transition of 35Cl16O4- (m/z 98.9) into 35Cl16O3- (m/z 82.9) was monitored for quantifying the main analyte; the transition of 37Cl16O4- (m/z 100.9) into 37Cl16O3- (m/z 84.9) was monitored for examining a proper isotopic abundance ratio of 35Cl/37Cl; and the transition of 35Cl18O4- (m/z 107.0) into 35Cl18O3- (m/z 89.0) was monitored for quantifying the internal standard. The minimum detection limit (MDL) for this method in de-ionized water is 5 ng l(-1) (ppt) using the API 2000 mass spectrometer and 0.5 ng l(-1) using the API 3200 mass spectrometer. Over 350 food and beverage samples were analyzed mostly in triplicate. Except for four, all samples were found to contain measurable amounts of perchlorate. The levels found ranged from 5 ng l(-1) to 463.5+/-6.36 microg kg(-1) using MRM 98.9-->82.9 and 100 microl injection.
已开发出一种新的离子色谱-电喷雾串联质谱(IC-ESI-MS/MS)方法,其样品前处理步骤简单,可用于定量和确证水、新鲜及罐装食品、葡萄酒和啤酒样品中低至万亿分之一(纳克/升,ng l⁻¹)水平的高氯酸盐(ClO₄⁻)阴离子。据我们所知,这是首次将一种分析方法用于测定葡萄酒和啤酒样品中的高氯酸盐。IC-ESI-MS/MS仪器由一台ICS-2500离子色谱(IC)系统与一台API 2000或API 3200质谱仪联用组成。对IC-ESI-MS/MS系统进行了优化,以监测两对前体离子和碎片离子的跃迁,即多反应监测(MRM)。所有样品在萃取前均添加了氧-18同位素标记的高氯酸盐内标(ISTD)。氯同位素比(³⁵Cl/³⁷Cl)用作确证工具。监测³⁵Cl¹⁶O₄⁻(质荷比98.9)到³⁵Cl¹⁶O₃⁻(质荷比82.9)的跃迁以定量主要分析物;监测³⁷Cl¹⁶O₄⁻(质荷比100.9)到³⁷Cl¹⁶O₃⁻(质荷比84.9)的跃迁以检查³⁵Cl/³⁷Cl的合适同位素丰度比;监测³⁵Cl¹⁸O₄⁻(质荷比107.0)到³⁵Cl¹⁸O₃⁻(质荷比89.0)的跃迁以定量内标。使用API 2000质谱仪时,该方法在去离子水中的最低检测限(MDL)为5 ng l⁻¹(ppt),使用API 3200质谱仪时为0.5 ng l⁻¹。分析了350多个食品和饮料样品,大多为一式三份。除了4个样品外,所有样品均检测到含有可测量的高氯酸盐。使用MRM 98.9→82.9和100微升进样时,检测到的含量范围为5 ng l⁻¹至463.5±6.36微克/千克(μg kg⁻¹)。