Journal of Forensic Medicine ›› 2024, Vol. 40 ›› Issue (6): 578-581.DOI: 10.12116/j.issn.1004-5619.2024.340603
Special Issue: 高分辨质谱技术专题
• Topic on High Resolution Mass Spectrometry Technology • Previous Articles Next Articles
Received:2024-06-12
Online:2025-03-10
Published:2024-12-25
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URL: http://www.fyxzz.cn/EN/10.12116/j.issn.1004-5619.2024.340603
| 时间/min | 流动相A | 流动相B |
|---|---|---|
| 0 | 90% | 10% |
| 4 | 90% | 10% |
| 14 | 2% | 98% |
| 24 | 2% | 98% |
| 24.1 | 90% | 10% |
| 30 | 90% | 10% |
Tab. 1 Gradient elution procedure
| 时间/min | 流动相A | 流动相B |
|---|---|---|
| 0 | 90% | 10% |
| 4 | 90% | 10% |
| 14 | 2% | 98% |
| 24 | 2% | 98% |
| 24.1 | 90% | 10% |
| 30 | 90% | 10% |
Fig. 1 Chromatograms and secondary mass spectra of yunaconitine and Bullatine B
Fig. 2 Extracted ion chromatogram （m/z 690.348 4）， primary mass spectrum and secondary mass spectrum ofsuspicious chromatographic peak in medicinal liquor
Fig. 3 Structural formula of pseudaconitine
| 碎片离子编号 | 元素组成 | 裂解途径 | 精确分子质量 | ||
|---|---|---|---|---|---|
| 理论值（m/z） | 实测值（m/z） | 相对偏差/×10-6 | |||
| 1 | C36H52NO12+ | ［M+H］+ | 690.348 4 | 690.349 4 | 1.4 |
| 2 | C35H46NO10+ | ［M+H-CH3OH-H2O］+ | 640.311 6 | 640.310 8 | -1.2 |
| 3 | C34H48NO10+ | ［M+H-AcOH］+ | 630.327 3 | 630.324 5 | -4.4 |
| 4 | C34H46NO9+ | ［M+H-AcOH-H2O］+ | 612.316 7 | 612.315 7 | -1.6 |
| 5 | C33H44NO9+ | ［M+H-AcOH-CH3OH］+ | 598.301 1 | 598.299 3 | -2.9 |
| 6 | C33H42NO8+ | ［M+H-AcOH-CH3OH-H2O］+ | 580.290 5 | 580.289 1 | -2.4 |
| 7 | C32H40NO8+ | ［M+H-AcOH-2CH3OH］+ | 566.274 8 | 566.274 0 | -1.5 |
| 8 | C9H9O3+ | ［M+H-C27H43NO9］+ | 165.054 6 | 165.054 5 | -0.9 |
Tab. 2 The elemental composition， fragmentation pathways， exact molecular mass andrelative deviation of suspicious compound
| 碎片离子编号 | 元素组成 | 裂解途径 | 精确分子质量 | ||
|---|---|---|---|---|---|
| 理论值（m/z） | 实测值（m/z） | 相对偏差/×10-6 | |||
| 1 | C36H52NO12+ | ［M+H］+ | 690.348 4 | 690.349 4 | 1.4 |
| 2 | C35H46NO10+ | ［M+H-CH3OH-H2O］+ | 640.311 6 | 640.310 8 | -1.2 |
| 3 | C34H48NO10+ | ［M+H-AcOH］+ | 630.327 3 | 630.324 5 | -4.4 |
| 4 | C34H46NO9+ | ［M+H-AcOH-H2O］+ | 612.316 7 | 612.315 7 | -1.6 |
| 5 | C33H44NO9+ | ［M+H-AcOH-CH3OH］+ | 598.301 1 | 598.299 3 | -2.9 |
| 6 | C33H42NO8+ | ［M+H-AcOH-CH3OH-H2O］+ | 580.290 5 | 580.289 1 | -2.4 |
| 7 | C32H40NO8+ | ［M+H-AcOH-2CH3OH］+ | 566.274 8 | 566.274 0 | -1.5 |
| 8 | C9H9O3+ | ［M+H-C27H43NO9］+ | 165.054 6 | 165.054 5 | -0.9 |
Fig. 4 Fragmentation pathways of pseudaconitine in mass spectrum
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