气相色谱-静电场轨道阱高分辨质谱法测定人血浆中7种甲基硅氧烷
Determination of seven methylsiloxanes in human plasma by gas chromatography-Orbitrap high-resolution mass spectrometry
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摘要:目的 基于液液萃取和气相色谱-静电场轨道阱高分辨质谱(GC-Orbitrap-MS)分析方法, 准确、快速地测定人血浆中7种甲基硅氧烷的浓度。方法 根据目标物质的理化性质, 对仪器分析条件和前处理条件进行优化。取100 μL人血浆样本加入甲醇以沉淀蛋白, 正己烷震荡萃取, 提取液使用真空离心浓缩机浓缩富集后, 采用TG-5HT色谱柱进行分离, 在电子轰击源(EI)模式下检测, 使用内标法进行定量。结果 7种甲基硅氧烷在1.56~50.00 μg/L的浓度范围内, 回归方程具备良好的线性关系, 决定系数(R2)> 0.995, 方法检出限范围为0.14~0.47 μg/L。在3个不同浓度水平下, 加标回收率范围为76.69%~122.65%, 相对标准偏差均小于15%。应用该方法对62份血样进行检测并定量分析显示, 共检出4种甲基硅氧烷, 浓度范围为 < LOD~36.22 μg/L。结论 本方法可同时检测人体血浆中7种甲基硅氧烷, 且准确性和灵敏度高, 适合大批量血浆样本中甲基硅氧烷的分析检测。Abstract:Objective To develop a precise and rapid method for determining the concentrations of seven methylsiloxanes in human plasma using liquid-liquid extraction combined with gas chromatography-Orbitrap high-resolution mass spectrometry (GC-Orbitrap-MS).Methods The analytical conditions of the instruments and pretreatment conditions were optimized based on the physicochemical properties of the target compounds. A 100 μL human plasma sample was mixed with methanol to precipitate proteins, followed by shake extraction with n-hexane. The extracts were concentrated using a centrifugal vacuum concentrator and then separated through a TG-5HT chromatographic column. Detection was performed in electron ionization mode, and quantification was carried out using the internal standard method.Results The seven methylsiloxanes showed good linear relationships in the concentration range of 1.56 to 50.00 μg/L, with coefficients of elemination (R2)>0.995. The limit of detection (LOD) ranged from 0.14 to 0.47 μg/L. Across three different concentrations, the spike recovery rates were 76.69% to 122.65%, and the relative standard deviations were all less than 15%. Applying this method to 62 blood samples for detection and quantitative analysis, a total of four methylsiloxanes were detected, with the concentrations ranging from < LOD to 36.22 μg/L.Conclusion This method allows for simultaneous detection of seven methylsiloxanes in human plasma with high accuracy and sensitivity. It is well-suited for methylsiloxane detection in large batches of human plasma samples.
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