کد مقاله | کد نشریه | سال انتشار | مقاله انگلیسی | نسخه تمام متن |
---|---|---|---|---|
7612893 | 1493570 | 2014 | 10 صفحه PDF | دانلود رایگان |
عنوان انگلیسی مقاله ISI
Fast liquid chromatographic-tandem mass spectrometric method using mixed-mode phase chromatography and solid phase extraction for the determination of 12 mono-hydroxylated brominated diphenyl ethers in human serum
ترجمه فارسی عنوان
روش سریع اسپکترومتر مایع کروماتوگرافی-دوبعدی با استفاده از کروماتوگرافی فاز فیزیکی مخلوط و استخراج فاز جامد برای تعیین 12 دیفنیل اتر مونو هیدروکسیل شده برومند شده در سرم انسان
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کلمات کلیدی
موضوعات مرتبط
مهندسی و علوم پایه
شیمی
شیمی آنالیزی یا شیمی تجزیه
چکیده انگلیسی
Hydroxylated polybrominated diphenyl ethers (OH-PBDEs) are formed from the oxidative metabolism of polybrominated diphenyl ethers (PBDEs) in humans, rats and mice, but their quantitation in human blood and other matrices with liquid chromatography-mass spectrometric techniques has been a challenge. In this study, a novel analytical method was developed and validated using only 250 μL of human serum for the quantitation of twelve OH-PBDEs, fully chromatographically separated in a 15 min analytical run. This method includes two novel approaches: an enzymatic hydrolysis procedure and a chromatographic separation using a mixed mode chromatography column. The enzymatic hydrolysis (EH) was found critical for 4â²-OH-BDE17, which was not detectable without it. For the sample clean up, a solid phase extraction protocol was developed and validated for the extraction of the 12 congeners from human serum. In addition, for the first time baseline resolution of two components was achieved that correspond to a single peak previously identified as 6â²-OH-BDE99. The method was validated for linearity, accuracy, precision, matrix effects, limit of quantification, limit of detection, sample stability and overall efficiency. Recoveries (absolute and relative) ranged from 66 to 130% with relative standard deviations <21% for all analytes. Limit of detection and quantitation ranged from 4 to 90 pg mLâ1 and 6-120 pg mLâ1, respectively, with no carry over effects. This method was applied in ten commercially available human serum samples from the general US population. The mean values of the congeners detected in all samples are 4â²-OH-BDE17 (34.2 pg mLâ1), 4-OH-BDE42 (33.9 pg mLâ1), 5-OH-BDE47 (17.5 pg mLâ1) and 4â²-OH-BDE49 (12.4 pg mLâ1).
ناشر
Database: Elsevier - ScienceDirect (ساینس دایرکت)
Journal: Journal of Chromatography A - Volume 1356, 22 August 2014, Pages 138-147
Journal: Journal of Chromatography A - Volume 1356, 22 August 2014, Pages 138-147
نویسندگان
Syrago-Styliani E. Petropoulou, Wendy Duong, Myrto Petreas, June-Soo Park,