Simultaneous quantitation of parabens, triclosan, and methyl triclosan in indoor house dust using solid phase extraction and gas chromatography-mass spectrometry
Simultaneous quantitation of parabens, triclosan, and methyl triclosan in indoor house dust using solid phase extraction and gas chromatography-mass spectrometry
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DOI：
10.1039/c0em00189a
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发表时间：
2010-01-01
影响因子：
--
通讯作者：
Jones-Otazo, Heather
中科院分区：
文献类型：
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作者：
Fan, Xinghua;Kubwabo, Cariton;Jones-Otazo, Heather
建立了基于气相色谱-质谱联用技术（GC/MS）同时测定室内灰尘中五种对羟基苯甲酸酯（甲基、乙基、丙基、丁基和苄基）、三氯生和甲基三氯生的分析方法。通过超声处理从灰尘样品中提取分析物。通过固相萃取 (SPE) 净化样品后，提取物用 N-甲基-N-(三甲基甲硅烷基) 三氟乙酰胺 (MSTFA) 衍生化，然后通过气相色谱法结合多反应监测 (MRM) 模式下的离子阱质谱进行分析。为了定量，对每个相应的目标分析物使用同位素标记的内标。分析仅需 0.05 克灰尘样品。方法检测限范围为 6.5 至 10 ng/g，绝对回收率为 74% 至 92%。所开发的方法表现出良好的重复性和重现性，所有分析物的相对标准偏差 (RSD) 均小于 16%。使用两种真空采样方法从 63 个加拿大家庭收集的灰尘样品中测定了分析物：使用 Pullman-Holt 真空采样器收集的新鲜或“活性”灰尘 (FD) 样品，以及从家用真空吸尘器 (HD) 中采集的复合样品。在所有 HD 和 FD 样品中均检测到对羟基苯甲酸甲酯、对羟基苯甲酸丙酯和三氯生。HD 样品产生中位数 对羟基苯甲酸甲酯、对羟基苯甲酸丙酯和三氯生的值分别为 1080、463 和 378 ng/g，与 FD 样品中值 1120、618 和 571 ng/g 相当。 FD 样品中对羟基苯甲酸乙酯的检出率为 89%，HD 样品中检出率为 73%，中位值分别为 52 ng/g 和 25 ng/g。丁基 FD 样品中对羟基苯甲酸酯的检测频率为 44%，HD 样品中检测到对羟基苯甲酸酯的频率为 75%，中位值为
An integrated analytical method for the simultaneous determination of five parabens (methyl-, ethyl-, propyl-, butyl-, and benzyl-), triclosan, and methyl triclosan in indoor house dust was developed based on gas chromatographic-mass spectrometric technique (GC/MS). Analytes were extracted from dust samples by sonication. After sample cleanup by solid-phase extraction (SPE), the extracts were derivatized with N-methyl-N-(trimethylsilyl) trifluoroacetamide (MSTFA) and then analyzed by gas chromatography coupled with ion trap mass spectrometry operated in multiple reaction monitoring (MRM) mode. For quantitation, isotope-labelled internal standards were used for each corresponding target analyte. Only 0.05 g of dust sample was needed for the analysis. Method detection limits ranged from 6.5 to 10 ng/g, and absolute recoveries from 74% to 92%. The developed method demonstrated good repeatability and reproducibility, with relative standard deviations (RSDs) less than 16% for all the analytes. The analytes were determined in dust samples collected using two vacuum sampling methods from 63 Canadian homes: a sample of fresh or "active'' dust (FD) collected using a Pullman-Holt vacuum sampler, and a composite sample taken from the household vacuum cleaner (HD). Methyl paraben, propyl paraben, and triclosan were detected in all HD and FD samples. HD samples yielded median values for methyl paraben, propyl paraben, and triclosan of 1080, 463, and 378 ng/g, respectively, which were comparable to the FD sample medians of 1120, 618 and 571 ng/g. Ethyl paraben was detected at frequencies of 89% in FD and 73% in HD samples, with median values of 52 and 25 ng/g, respectively. Butyl paraben was detected at frequencies of 44% in FD and 75% in HD samples, with median values of