Machida Koichi, Kotani Akira, Hayashi Yuzuru, Hakamata Hideki
School of Pharmacy, Tokyo University of Pharmacy and Life Sciences, Tokyo, Japan.
Institute for FUMI Theory, Chiba, Japan.
J Mass Spectrom. 2022 Aug;57(8):e4877. doi: 10.1002/jms.4877.
ISO 11843 part 7 (ISO 11843-7) can provide a standard deviation (SD) of area measurements of a target peak through the stochastic behaviors of instrumental noises. The purpose of this study is to demonstrate that ISO 11843-7 can be applied to assess repeatability in an isocratic liquid chromatography-tandem mass spectrometry (LC-MS/MS) system without repetitive measurements. The relative standard deviation (RSD) of the peak area of ergosterol picolinyl ester, which was used as an example, on a multiple reaction monitoring (MRM) chromatogram was determined by ISO 11843-7. The RSD by ISO 11843-7 (N = 1) was within a 95% confidence band of the RSD by repetitive measurements (N = 6). Moreover, the effects of digital smoothing, such as moving average, were also examined on the repeatability assessment in LC-MS/MS by ISO 11843-7. From the results of the comparisons of the RSDs obtained by ISO 11843-7 and the repetitive measurements, it was shown that suitable RSDs of the peak area were obtained from the smoothed MRM chromatograms by the moving average for narrow data point windows (e.g., one-sixth of the peak width). In conclusion, the utility of repeatability assessment based on ISO 11843-7 has been expanded for the validation of an LC-MS/MS system.
ISO 11843第7部分（ISO 11843-7）可通过仪器噪声的随机行为提供目标峰面积测量的标准偏差（SD）。本研究的目的是证明ISO 11843-7可用于评估等度液相色谱-串联质谱（LC-MS/MS）系统中的重复性，而无需进行重复测量。以麦角甾醇吡啶酯为例，通过ISO 11843-7测定了多反应监测（MRM）色谱图上峰面积的相对标准偏差（RSD）。ISO 11843-7（N = 1）得到的RSD在重复测量（N = 6）得到的RSD的95%置信区间内。此外，还研究了数字平滑（如移动平均）对ISO 11843-7在LC-MS/MS重复性评估中的影响。通过比较ISO 11843-7和重复测量得到的RSD结果表明，对于窄数据点窗口（例如，峰宽的六分之一），通过移动平均从平滑后的MRM色谱图中获得了合适的峰面积RSD。总之，基于ISO 11843-7的重复性评估的实用性已扩展到LC-MS/MS系统的验证。
