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  • Title: [Determination of polybrominated diphenyl ethers in serum using isotope internal standard-gas chromatography-high resolution dual-focus magnetic mass spectrometry].
    Author: Wang M, Xie L, Zhu Y, Lu Y.
    Journal: Se Pu; 2022 Apr; 40(4):354-363. PubMed ID: 35362683.
    Abstract:
    A method for the determination of 14 polybrominated diphenyl ethers (PBDEs) in human serum using isotope internal standard-gas chromatography-high resolution dual-focus magnetic mass spectrometry (GC-HRMS) was developed. After thawed to room temperature, 0.5 mL serum samples were mixed with 13C-labeled isotopic internal standard. Subsequently, methanol was added to precipitate the proteins in the samples. The effects of three kinds of acids on the removal of cellulite from the serum samples and the corresponding recoveries were compared, and the results revealed that sulfuric acid was the most optimal. The target compounds were extracted by liquid-liquid extraction (LLE), and the effects of different extraction solvents on recoveries were compared. The results indicated that n-hexane (6 mL)-methyl tert-butyl ether (6 mL) was the best extraction solvent. The extracts were cleaned and eluted using solid phase extraction cartridges. Furthermore, the factors that influenced the cleanup effects and recoveries, including the solid phase extraction columns and elution solvents, were investigated in detail. The results indicated that the optimal conditions were cleanup with a silica gel column and elution with hexane-dichloromethane (1∶1, v/v). The eluate was re-dissolved in hexane after being blown to near dryness using nitrogen. The detection of PBDEs was performed using GC-HRMS. The instrument conditions were optimized, and the capillary column used was an Rtx-1614 column (30 m×0.25 mm×0.1 μm). Helium was used as the carrier gas at a flow rate of 1.0 mL/min. The injector temperature was 290 ℃, and the oven temperature was programmed as follows: 150 ℃ for 2 min, 150 ℃ to 250 ℃ at 15 ℃/min, held for 1 min, 250 ℃ to 290 ℃ at 25 ℃/min, held for 3 min, and 290 ℃ to 320 ℃ at 25 ℃/min, held for 12.5 min. The injection volume was 1 μL in splitless mode. The samples were ionized in the positive electron ionization (EI) mode at 35 eV. Precursor ions and the production of each compound were identified using a voltage-selective ion detection (VSIR) program with a resolution of 10000. The ionization temperature was set at 280 ℃, and the transmission line temperature was set at 320 ℃. To ensure the integrity of the separation of low-brominated components, the column separation time was shortened, the response of high-boiling components was improved (BDE-190 and BDE-209), the decomposition of BDE-209 on the chromatographic column was effectively prevented, and the requirement of the simultaneous determination of multiple PBDEs was met. The method demonstrated good linearity in the range of 0.40 to 25 μg/L for BDE-209, and 0.08 to 5 μg/L for the other 13 PBDEs, with correlation coefficients greater than 0.995. The method detection limits (MDLs) were in the range of 0.01 to 0.51 μg/L, and the limits of quantification (LOQs) ranged from 0.04 to 1.70 μg/L. The recoveries of the 14 compounds ranged from 75.5% to 120.7%. The intra-day relative standard deviations (RSDs) were within 3.8%-10.9% (n=6) and the inter-day RSDs were within 4.2% to 12.4% (n=6). This method was successfully applied to the determination of 14 PBDEs in 15 serum samples from an adolescent population in an area. Notably, 1.86 to 4.66 ng/g lipid BDE-47 was detected in the serum samples with a detection frequency of 100%, and the other compounds were not detected. The results imply that the adolescent population in this region was exposed to some PBDE. Compared with the existing methods reported, this method has less sample demand and higher sensitivity and accuracy, can simultaneously determine 14 PBDEs, including BDE-209 in human serum, and effectively improve the efficiency of detection. This study offers a new method for studying the impact of polybrominated diphenyl ethers on population health in China. 建立了同位素内标-气相色谱-高分辨双聚焦磁质谱(GC-HRMS)同时测定人体血清中14种多溴联苯醚(PBDEs)的方法。血清样品解冻后,取0.5 mL与13C标记的内标物进行混合,加入甲醇沉淀样品中的蛋白质,比较了3种酸化条件下的去脂效果和回收率,结果显示硫酸去脂效果最好;使用液液萃取法提取样品中的目标物,比较了不同萃取溶剂对回收率的影响,结果显示以正己烷(6 mL)-甲基叔丁基醚(6 mL)作为萃取溶剂效果最好;提取液经固相萃取柱净化和洗脱,比较了不同固相萃取柱和洗脱溶剂的净化效果和回收率,结果显示采用硅胶柱净化和用正己烷-二氯甲烷(1:1, v/v)洗脱时效果最好;洗脱液经氮吹近干后用正己烷复溶,经GC-HRMS测定。目标物经Rtx-1614色谱柱(30 m×0.25 mm×0.1 μm)分离,电压选择离子检测(VSIR)模式测定。BDE-209在0.40~25 μg/L、其他13种多溴联苯醚在0.08~5 μg/L范围内线性关系良好,相关系数>0.995,方法检出限为0.01~0.51 μg/L,定量限为0.04~1.70 μg/L,加标回收率为75.5%~120.7%,日内精密度为3.8%~10.9%(n=6),日间精密度为4.2%~12.4%(n=6)。应用该方法对采集的某地区15份青少年血清样本进行检测,结果显示14种PBDEs中,BDE-47检出率为100%,其他组分均未检出,说明该人群存在一定的PBDEs暴露。与现有文献报道方法相比,本方法样本需求量少,灵敏度、准确度较高,可对人血清中包括BDE-209在内的14种PBDEs同时测定,有效提高检测效率。本方法的建立可为我国开展多溴联苯醚对人群健康的影响提供技术支撑。
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