Dionex Corporation, Sunnyvale, CA 94085, USA.
Rapid Commun Mass Spectrom. 2010 Sep 15;24(17):2605-10. doi: 10.1002/rcm.4679.
A high-throughput method was developed for the direct analysis of trace level bisphenol A (BPA), 4-n-octylphenol (4-n-OP), 4-tert-octylphenol (4-t-OP) and 4-n-nonylphenol (4-n-NP) in water samples by ultra-high-performance liquid chromatography/tandem mass spectrometry (uHPLC/MS/MS) using an isotope-labeled internal standard. Aliquots of water samples were spiked with the internal standard and analyzed without sample cleanup or enrichment. All target analytes were chromatographically separated within 3 min and detected using the highly selective multiple reaction monitoring (MRM) detection mode. The method detection limits were statistically calculated and ranged from 0.040 ppb (BPA) to 0.057 ppb (4-n-NP). Excellent correlation of determination was achieved for each analyte with r greater than 0.995. Precision was achieved within 8% relative standard deviation (RSD) for all analytes, and recoveries from spiked samples ranged from 97% to 106.2% except for 4-n-OP which may be corrected by using an isotope-labeled analog as internal standard. This method was used for analyzing eight randomly selected bottled water samples and found no detectable target analytes. This method was also used to analyze target analytes leached from bottles (6 low cost bottles and 6 brand-name baby-feeding bottles). Low levels of BPA were found in three bottles after they had been heated in a microwave oven, and a trace amount of 4-n-NP was also found in three bottles. 4-t-OP, which has not been reported as a leachable chemical, was found in two brand name baby-feeding bottles from the same manufacturer, and was confirmed with bottles from different batches.
建立了一种超高效液相色谱/串联质谱法(uHPLC/MS/MS),通过同位素标记内标,直接分析水样中痕量水平的双酚 A(BPA)、4-正辛基酚(4-n-OP)、4-叔辛基酚(4-t-OP)和 4-正壬基酚(4-n-NP)。水样经同位素标记内标处理后,不经样品净化或富集直接分析。所有目标分析物在 3 分钟内实现色谱分离,并采用高度选择性的多重反应监测(MRM)检测模式进行检测。通过统计计算得出方法检测限,范围为 0.040 ppb(BPA)至 0.057 ppb(4-n-NP)。每个分析物的相关性均大于 0.995。除 4-n-OP 外,所有分析物的精密度均在 8%相对标准偏差(RSD)范围内,加标回收率在 97%至 106.2%之间,4-n-OP 可能需要通过使用同位素标记的类似物作为内标进行校正。该方法用于分析 8 个随机选择的瓶装水样品,未检出目标分析物。该方法还用于分析从瓶中浸出的目标分析物(6 个低价瓶和 6 个名牌婴儿奶瓶)。发现三个经微波炉加热的瓶子中存在低水平的 BPA,三个瓶子中也检测到痕量的 4-n-NP。4-t-OP 未被报道为可浸出的化学物质,但在同一制造商的两个名牌婴儿奶瓶中发现,在来自不同批次的奶瓶中也得到了证实。