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目的:鉴定碘海醇中保留时间在碘海醇外异构体之后的有关物质。方法:采用Sycronis C_(18)(100 mm×2.1 mm,3.0μm)色谱柱,以0.01%甲酸水溶液为流动相A,甲醇为流动相B,梯度洗脱,采用基于静电场轨道阱(Orbitrap)技术的质谱法,根据精确分子量和一级、二级裂解规律,对保留时间在碘海醇之后有关物质的色谱峰进行质谱分析。结果:精确分子量表明,这些有关物质或是O-烷基化合物或是N-烷基化合物;裂解规律表明,O-烷基化合物更容易形成m/z 803.877 0碎片离子和m/z 166.107 38碎片离子;N-烷基化合物可形成m/z 112.075 69、m/z 104.070 60和m/z 86.060 04碎片离子;据此推测出有关物质1~5为N-烷基化化合物,有关物质6~11为O-烷基化合物。结论:研究结果可为碘海醇质量标准修订和检测结果的判断提供科学、合理和可靠的依据。
OBJECTIVE: To identify the related substances in iohexol after retention time of iohexol external isomer. METHODS: Sycronis C 18 column (100 mm × 2.1 mm, 3.0 μm) was used. The mobile phase A was consisted of 0.01% formic acid in water and the mobile phase B was methanol. The mobile phase was gradient elution. Electron field Orbitrap Technology mass spectrometry, according to the accurate molecular weight and the primary and secondary cleavage laws, the retention time after iohexol related substances chromatographic peak mass spectrometry. Results: The exact molecular weights indicated that these related substances were either O-alkyl compounds or N-alkyl compounds; the cleavage pattern showed that O-alkyl compounds were more likely to form m / z 803.877 0 fragment ions and m / z 166.107 38 fragments Ions; N-alkyl compounds can form m / z 112.075 69, m / z 104.070 60 and m / z 86.060 04 fragment ions; it is inferred that related substances 1 to 5 are N-alkylated compounds, 11 is an O-alkyl compound. Conclusion: The results of this study can provide a scientific, reasonable and reliable basis for the revision of iohexol standard and the determination of test results.