Spatial correlation spectrum testing method of cephalomannine based on nuclear magnetic resonance technology

A mannine and space-related technology, which is applied in the directions of analysis by nuclear magnetic resonance, material analysis by resonance, and measurement devices to achieve the effect of optimizing relevant parameters

Active Publication Date: 2020-09-15
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It is an ideal technique to solve the three-dimensional structure of medium-sized compounds, but there are two problems in ROESY technology: one is how to suppress similar two-dimensional NMR signals, so as not to affect the identification of ROESY signals; the other is how to eliminate the off-resonance effect. Impact
[0006] At present, there is no report on the test method of cephalomannine spatial correlation spectrum (ROESY), but there are some methods for the separation of cephalomannine and paclitaxel, cephalomannine derivatives and their preparation methods, and their drug combinations Reports on substances and uses, preparation of 10-deacetylbaccatin by hydrolysis of cephalomannine base, etc.

Method used

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  • Spatial correlation spectrum testing method of cephalomannine based on nuclear magnetic resonance technology
  • Spatial correlation spectrum testing method of cephalomannine based on nuclear magnetic resonance technology
  • Spatial correlation spectrum testing method of cephalomannine based on nuclear magnetic resonance technology

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Embodiment 1

[0032] The method proposed in the present invention is used to determine the ROESY spectrum of cephalomannine as an example, and this specific example is used to verify the feasibility of the present invention in determining the ROESY spectrum of cephalomannine. The sample used in the experiment was cephalomannine, and the experimental test was carried out under an Agilent 600MHz NMR spectrometer (Agilent, USA). The whole experimental process did not carry out any sample pretreatment on the sample, and did not change the hardware facilities of the instrument. According to the operation process of the method proposed in the present invention, the concrete steps are as follows:

[0033] Step 1, weigh the sample and put it into a test tube, add the deuterated solvent DMSO, dissolve it fully by ultrasonic, transfer it to the nuclear magnetic tube, and then put the test tube with the sample into the detection magnet of the nuclear magnetic spectrometer;

[0034] Step 2, select the ...

Embodiment 2

[0045] As shown in Table 1, the present embodiment optimizes the mixing time (mixR) on the basis of Example 1, respectively setting the mixing time (mixR) as 100ms, 200ms, 300ms, 400ms, 500ms and finding that when mixR is 400ms, The number of measured ROE correlation points is the largest and basically stable, so it is preferable to set mixR to 400ms.

[0046] Table 1 The signal corresponding table of the ROESY spectrum of the samples at different mixing times (mixR)

[0047]

[0048]

Embodiment 3

[0050] As shown in Table 2, in this embodiment, according to the detected direct dimensional spectral width sw is 6313Hz, on the basis of embodiment 1, the sampling time at of the sampling period is adjusted, from 100ms to 150ms, 200ms, and the measured ROE The large change in the number of relevant points indicates that the optimization of the sampling time is more effective, so the optimal sampling time at is 150ms.

[0051] Table 2 Signal correspondence table of ROESY spectrum of samples at different sampling times (at)

[0052] serial number Sampling time (ms) The number of ROE correlation points 1 at=100 12 2 at=150 15 3 at=200 13

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Abstract

The invention relates to the field of chemical analysis, in particular to a nuclear-magnetic-resonance-technology-based spatial correlation spectrum (ROESY) test method for cephalomannine. According to the invention, on the basis of the optimized design of a pulse sequence, a spatial correlation spectrum ROESY of cephalomannine is measured by using hydrogen as an observation nucleus. At present, most of spatial correlation spectrums used by instruments are based on the NOESY spectrum and the NOE signals for some medium molecules are zero, so that the spatial correlation conditions can not be characterized by using the NOESY. On the basis of the characteristics of the molecules of cephalomannine, the ROESY spectrum is introduced based on concept changing and the relevant parameters are optimized. Therefore, the defect of weak NOE signal is overcome; and the an effective and simple means for characterizing the spatial structure for medium-sized molecules is provided.

Description

technical field [0001] The invention relates to the field of chemical analysis, in particular to a test method based on nuclear magnetic resonance technique spatial correlation spectrum (ROESY). Background technique [0002] Cephalomannine is derived from Taxus chinensis. It is an important pharmaceutical intermediate, material intermediate, and fine chemical, and has anti-inflammatory and anti-tumor effects. At the same time, cephalomannine can also be transformed into the important anti-tumor drug paclitaxel, the chemical structure is only the amide side chain is different, it can be used as an important raw material for the chemical synthesis of paclitaxel, and can be developed as a new type of taxane precursor. [0003] The structural formula of cephalomannine is as follows: [0004] [0005] In recent years, two-dimensional nuclear magnetic resonance spectroscopy has been applied to the determination and analysis of the spatial conformation of drug molecules in liq...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N24/08
CPCG01N24/087
Inventor 刘雅琴
Owner ZHEJIANG UNIV
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