College of Materials Science and Engineering, Chongqing University, Chognqing, 400045, PR China.
College of Materials Science and Engineering, Yangtze Normal University, Fuling, 408100, PR China.
Anal Chim Acta. 2021 Jun 22;1165:338564. doi: 10.1016/j.aca.2021.338564. Epub 2021 Apr 24.
This study proposes a new strategy to determine ultra-trace Ti in human serum using inductively coupled plasma tandem mass spectrometry (ICP-MS/MS). The human serum samples were diluted with 1% (v/v) HNO, followed by the determination of ultra-trace Ti using ICP-MS/MS. In the MS/MS mode, a small amount of H was mixed with O (the reaction gas) in a collision reaction cell (CRC) to form an O/H reaction mixture, and then, the conversion of Ti to TiO was determined by the O mass shift method. High concentrations of Ca, S, and P in human serum were ionized in plasma, and the formed Ca, SO, and PO reacted with O in CRC to form CaO, SO, and PO to interfere with the determination of TiO. We employed the mass shift reaction of H and oxide ions to eliminate this interference. This method was evaluated using the human serum sample spike recovery experiment and comparative analysis by sector field (SF)-ICP-MS. The results showed that using reaction gas mixture O/H reduced the background equivalent concentration (BEC) of Ti and improved sensitivity. The values determined by this method were consistent with the SF-ICP-MS values, which confirmed its accuracy and reliability. The limit of detection (LOD) of Ti was 0.78-7.20 ng L, the recovery was 96.0%-104%, and the relative standard deviation (RSD) was 2.0%-4.2%. This method has solved the problem that the determination of ultra-trace Ti in human serum cannot be accurately determined using O reaction mode. It realizes the interference-free and highly sensitive determination of the ultra-trace Ti in samples with high levels of Ca, S, and P and provides a new technique for high-throughput and accurate determination of ultra-trace Ti in human serum.
本研究提出了一种使用电感耦合等离子体质谱串联质谱法（ICP-MS/MS）测定人血清中超痕量钛的新策略。将人血清样品用 1%（v/v）HNO3 稀释，然后使用 ICP-MS/MS 测定超痕量钛。在 MS/MS 模式下，将少量 H 与 O（反应气）混合在碰撞反应池（CRC）中，形成 O/H 反应混合物，然后通过 O 质量位移法确定 Ti 向 TiO 的转化。人血清中高浓度的 Ca、S 和 P 在等离子体中被电离，形成的 Ca、SO 和 PO与 CRC 中的 O 反应，形成 CaO、SO 和 PO，干扰 TiO 的测定。我们采用 H 和氧化物离子的质量位移反应消除这种干扰。该方法通过人血清样品加标回收实验和扇形场（SF）-ICP-MS 比较分析进行评估。结果表明，使用反应气混合物 O/H 降低了 Ti 的背景等效浓度（BEC）并提高了灵敏度。该方法测定的结果与 SF-ICP-MS 的结果一致，证实了其准确性和可靠性。Ti 的检出限（LOD）为 0.78-7.20ng/L，回收率为 96.0%-104%，相对标准偏差（RSD）为 2.0%-4.2%。该方法解决了使用 O 反应模式无法准确测定人血清中超痕量钛的问题，实现了高钙、高硫、高磷样品中超痕量钛的无干扰、高灵敏度测定，为高通量、准确测定人血清中超痕量钛提供了一种新的技术。
