在使用NMR的药物成分中快速而简单的脂质量测量
Francesco Currò1,2,3, Ander Eguskiza3, Linda Cerofolini1,2,4
1Department of Chemistry Ugo Schiff (DICUS), University of Florence, via Della Lastruccia 3, 50019 Sesto Fiorentino, Italy.
ACS omega
|November 17, 2025
概括
核磁共振 (NMR) 光谱学,特别是PULCON方法,可以准确量化脂质体中的脂质. 这种快速的NMR技术非常适合制药制造业的质量控制.
科学领域:
- 制药科学 制药科学
- 分析化学 分析化学
- 材料科学 材料科学 材料科学
背景情况:
- 脂质体是药品中至关重要的纳米级输送系统.
- 精确的脂质量测量对于脂质体配方的质量和有效性至关重要.
- 现有的方法可能缺乏大规模制造所需的速度和一致性.
研究的目的:
- 评估核磁共振 (NMR) 光谱法,以精确量化脂质在脂质体.
- 评估PULCON (基于脉冲长度的度确定) 方法用于分析常见的脂质体脂质.
- 为了比较NMR量化与超高性能液态染色学与蒸发光散射检测 (UPLC-ELSD).
主要方法:
- 使用NMR光谱与内部参考和外部标准PULCON方法量化脂质.
- 脂质的分析包括DSPC,DOPC,胆固醇和DMPE-PEG2K.
- 用UPLC-ELSD对脂质体溶液进行比较分析.
主要成果:
- 内部和外部标准的PULCON NMR方法都显示出高准确性,精度和可重复性.
- 普尔康核磁共振技术提供了更高的一致性和更快的分析时间.
- 核磁共振量化结果与通过UPLC-ELSD获得的结果相似.
结论:
- 普尔康NMR光谱是一种可靠和高效的方法,用于脂质体中的脂质量定量.
- 普尔康NMR的速度和准确性使其适用于工业质量控制和配方优化.
- 这项研究支持开发用于制药制造的快速,准确的脂质量定量.
相关概念视频
00:52¹H NMR of Conformationally Flexible Molecules: Temporal Resolution
At room temperature, the chair conformer of cyclohexane undergoes rapid ring flipping between two equivalent chair conformers at a rate of approximately 105 times per second. These two chair conformers are in equilibrium. The rapid ring flipping results in the interconversion of the axial proton to an equatorial proton and an equatorial to the axial proton. Such interconversions are too rapid and cannot be detected on the NMR timescale. Hence, the NMR spectrometer cannot distinguish between the...
01:15NMR Spectroscopy and Mass Spectrometry of Aldehydes and Ketones
In aldehydes, the hydrogen atom connected to the carbonyl carbon helps distinguish aldehydes from other carbonyl compounds using ¹H NMR spectroscopy. The closeness of aldehydic hydrogen to the electrophilic carbonyl carbon highly deshields the hydrogen atom causing its signal to appear around 10 ppm in the ¹H NMR spectra. α hydrogens split the aldehydic proton signal, which helps identify the number of α hydrogens in the molecule. For instance, one α hydrogen creates a doublet for an aldehydic...
01:30NMR and Mass Spectroscopy of Carboxylic Acids
In ¹H NMR spectroscopy, acidic protons (–COOH) of carboxylic acids are highly deshielded and absorb far downfield, at around 9–12 ppm. The chemical shift value depends on the concentration and solvent used.
While α protons of carboxylic acids absorb at 2–2.5 ppm, β protons absorb further upfield.
Carboxylic acids are easily identified by dissolving them in deuterium oxide, which results in a rapid exchange of the acidic protons with deuterium. This leads to the disappearance of the acidic...
While α protons of carboxylic acids absorb at 2–2.5 ppm, β protons absorb further upfield.
Carboxylic acids are easily identified by dissolving them in deuterium oxide, which results in a rapid exchange of the acidic protons with deuterium. This leads to the disappearance of the acidic...
00:58¹H NMR Signal Integration: Overview
The intensity of a signal, which can be represented by the area under the peak, depends on the number of protons contributing to that signal. The area under each peak is shown as a vertical line called an integral, with the integral value listed under it, as seen in the proton NMR spectrum of benzyl acetate. Each integral value is divided by the smallest integral value to obtain the ratio of the number of protons producing each signal. The ratio reveals the relative number of protons and not...
01:25Applications Of NMR In Biology
Nuclear magnetic resonance (NMR) spectroscopy is a very valuable analytical technique for researchers. It has been used for more than 50 years as an analytical tool. F. Bloch and E. Purcell formulated NMR in 1946 and won the 1952 Nobel Prize in Physics for their work. Biological macromolecules such as proteins, nucleic acids, lipids, and organic molecules including pharmaceutical compounds, can be studied using this versatile tool that exploits the magnetic properties of certain nuclei.
The...
The...
01:17Chemical Shift: Internal References and Solvent Effects
In an NMR sample, precise measurement of the absolute absorption frequencies of nuclei is difficult. A standard internal reference compound is added, and the frequency difference between the reference signal and sample signals is measured.
The internal reference compound generally used in NMR spectroscopy is tetramethylsilane (TMS). TMS is preferred because it is chemically inert, soluble in NMR solvents, and easily removable. Also, the highly shielded methyl protons in TMS yield an intense...
The internal reference compound generally used in NMR spectroscopy is tetramethylsilane (TMS). TMS is preferred because it is chemically inert, soluble in NMR solvents, and easily removable. Also, the highly shielded methyl protons in TMS yield an intense...