Method for analyzing traditional Chinese medicine dimethyl sulfoxide extracting solution by nuclear magnetic resonance technology
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A dimethyl sulfoxide and nuclear magnetic resonance technology, applied in the direction of analysis by nuclear magnetic resonance, can solve the problems of loss, destruction and distortion of volatile components, and achieve the effects of short extraction time, avoidance of volatilization, and easy and safe operation.
Inactive Publication Date: 2011-08-10
周至譓
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Here, deuterated dimethyl sulfoxide is only used as an internal standard rather than an extractant. The water-soluble components or oil-soluble components extracted by other extractants are only some components of traditional Chinese medicine. The heat-sensitive, easily oxidized, easily hydrolyzed, and volatile The components in the extraction process may be destroyed, and the volatile components may also be lost with the evaporation of the extractant, and the resulting nuclear magnetic resonance spectrum may be incomplete and distorted
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Embodiment 1
[0013] Prepare the test solution, weigh Chinese medicinal materials or Chinese medicinal preparations according to the provisions of the "Chinese Pharmacopoeia", and carry out pretreatment, replace the original extraction agent with dimethyl sulfoxide according to the extraction dose specified under the same item, at a temperature of 25 ° C , extract by ultrasonic treatment for 30 minutes, and filter. If the viscosity of the extract is high, centrifugation can be used, and the supernatant is taken as the test solution. If the test product contains biological enzymes, proteins and other components that are easily oxidized, variable, or heat-sensitive, the solution of the test product should be prepared by percolation or impregnation.
[0014] This method is suitable for conventional one-dimensional tests: including hydrogen spectrum, carbon spectrum (including DEPT), oxygen spectrum, phosphorus spectrum, silicon spectrum, etc.; various two-dimensional spectrum tests: such as COZ...
Embodiment 2
[0020] Prepare the test solution, weigh Chinese herbal medicines or Chinese medicine preparations according to regulations, and carry out pretreatment, replace the original extractant with dimethyl sulfoxide according to the extraction dose specified under the same item, and ultrasonically treat for 15 minutes at a temperature of 18.45°C. Minute extraction, filtration, if the viscosity of the extract is high, centrifugation can be used, and the supernatant is taken as the test solution. Other steps and principles are the same as those in Embodiment 1.
Embodiment 3
[0022] Prepare the test solution, weigh the Chinese herbal medicine or Chinese medicine preparation according to the regulations, and carry out pretreatment, replace the original extractant with dimethyl sulfoxide according to the extraction dose specified under the same item, and ultrasonically treat it for 120 minutes at a temperature of 189 ° C Minute extraction, filtration, for the test solution. Other steps and principles are the same as in Embodiment 1, and this operation is applicable to traditional Chinese medicines such as Shicai Ming.
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Abstract
The invention relates to a method for analyzing traditional Chinese medicine dimethyl sulfoxide extracting solution by a nuclear magnetic resonance technology. The invention is characterized in that the method comprises the following steps: preparing sample solution, weighting traditional Chinese medicines or Chinese herbal preparation according to the regulation, carrying out pretreatment on the traditional Chinese medicines or the Chinese herbal preparation, using dimethyl sulfoxide to replace an original extracting agent according to the extraction dosage specified in the same item, extracting and filtering by an extraction method frequently-used for traditional Chinese medicine at the temperature of 18.45 DEG C to 189 DEG C to obtain the sample solution, adopting a conventional nuclear magnetic resonance system, selecting parameters of each system according to the nuclear magnetic resonance system and the characteristics of the traditional Chinese medicine, determining the content of the sample solution qualitatively and quantitatively, thereby obtaining a nuclear magnetic resonance spectrum containing all compositions of the traditional Chinese medicine, a molecular structure and physical characteristics. In the method, the dimethyl sulfoxide is used as the extracting agent for extracting the traditional Chinese medicines and the Chinese herbal preparation; the method can totally extract all water soluble, oil soluble, volatile compositions of the traditional Chinese medicine at the room temperature of over 18.45 DEG C by an ultrasonic method, can avoid the volatilization, hydrolyzation, oxidation, denaturation of active ingredients and preserves the bioactivity of the active ingredients to the greatest extent. The method is simple, convenient and safe to operate and has short extraction time.
Description
technical field [0001] The invention relates to a method, in particular to a method for analyzing Chinese medicine dimethyl sulfoxide extract by nuclear magnetic resonance technology. Background technique [0002] NMR technology is a spectroscopic method used to study the molecular structure and physical properties of substances, especially the reference of pulse Fourier transform NMR and superconducting NMR in recent years, two-dimensional, three-dimensional, solid high-resolution NMR spectra The emergence of NMR has improved the sensitivity and information content of NMR spectrometers, and has become an indispensable structural analysis tool for modern Chinese medicine research. [0003] At present, when NMR technology is used to determine the hydrogen spectrum and carbon spectrum of traditional Chinese medicine, the water-soluble components and oil-soluble components of traditional Chinese medicine are extracted with water, methanol, ether, acetone, n-butanol and other ex...
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