A cleanup method of serum extracts withmolecular sieves as SPE sorbents for the analysis of polybrominated diphenyl ethers
A cleanup method of serum extracts withmolecular sieves as SPE sorbents for the analysis of polybrominated diphenyl ethers
复制标题
DOI：
10.1002/jssc.202100889
复制
发表时间：
2022-06-23
影响因子：
3.1
通讯作者：
Hu，Chun
中科院分区：
文献类型：
--
作者：
Liu，Hongyuan;Jin，Jing;Hu，Chun
基于尺寸和形状选择性吸附，13X 分子筛被开发为固相萃取吸附剂，用于净化血清提取物，用于测定多溴二苯醚。研究了影响净化效率的重要参数，包括吸附剂的量、溶剂的类型和体积。在优化条件下，通过凝胶渗透色谱和气相色谱-质谱法评价去除杂质的能力。结果表明，净化后玉米油（13毫克）中高达99%的脂质可以被去除，血清中的内源性化合物也可以被有效消除。净化效率不仅优于亲水亲油平衡柱，而且接近酸性硅胶和多功能杂质吸附剂。一般来说，所开发的净化方法对于含有四个以上溴的多溴二苯醚表现出较高的回收率，特别是对于九溴和十溴二苯醚（99.1˗117.8%）。该净化方法可以与气相色谱法和串联质谱法结合用于人血清中的多溴二苯醚分析。除2,3',4',6-四溴二苯醚、2,3',4',6-五溴二苯醚和2,3,3',4,4',5',6-七溴二苯醚外,方法检出限为0.01˗0.27 ng/mL,平均回收率为50.9˗113.3%。 2,2',4,5'-四溴二苯醚在人血清中的检测频率最高（95%），而十溴二苯醚的平均浓度最大（0.50 ng/mL）。
Based on the size‐ and shape‐selective sorption, 13X molecular sieves were developed as solid‐phase extraction adsorbents to cleanup serum extract for the determination of polybrominated diphenyl ethers. The important parameters affecting the cleanup efficiency were investigated including the amount of sorbents, the type, and volume of solvents. Under the optimized conditions, the capacity for removing impurities was evaluated via gel permeation chromatography and gas chromatography with mass spectrometry. The results demonstrated that up to 99% of lipids in corn oil (13 mg) can be removed after cleanup, and endogenous compounds in serum can also be effectively eliminated. The cleanup efficiency is not only superior to hydrophile‐lipophile balance column, but also close to acid silica gel and multifunction impurity sorbents. Generally, the developed cleanup method exhibited higher recovery for polybrominated diphenyl ethers with more than four bromines, especially for nona‐ and deca‐brominated diphenyl ethers (99.1˗117.8%). The cleanup method can be coupled with gas chromatography and tandem mass spectrometry for polybrominated diphenyl ethers analysis in human serum. The method detection limits were 0.01˗0.27 ng/mL and average recovery was 50.9˗113.3%, except 2,3',4',6‐tetrabrominated, 2,3',4,4',6‐pentabrominated, and 2,3,3',4,4',5',6‐heptabrominated diphenyl ethers. 2,2',4,5'‐Tetrabrominated diphenyl ethers had the highest detection frequency (95%) in human serum, whereas decabrominated diphenyl ethers had the maximum mean concentration (0.50 ng/mL).