Preparation method of phorbol ester compound Euphorbia Factor L1

A technology of ester compound and Qianjinzi, which is applied in the field of preparation of diterpene alcohol ester compound Qianjinzi No. 1, can solve the problems of life-threatening, toxic and side effects, sequelae, iatrogenic diseases and the like

Active Publication Date: 2015-03-25
TIANJIN LANGLI PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Malignant tumor is a serious disease with unknown cause. At present, surgery, radiotherapy, and chemotherapy are the main methods. Surgery is mostly suitable for early cancer patients. Radiotherapy and chemotherapy are only effective for

Method used

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  • Preparation method of phorbol ester compound Euphorbia Factor L1
  • Preparation method of phorbol ester compound Euphorbia Factor L1
  • Preparation method of phorbol ester compound Euphorbia Factor L1

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Preparation of Diterpene Alcohol Esters (QJZ-6)

[0032] 1. Obtaining the primary extract of QJZ-6

[0033] 1. Crushing:

[0034] Take Qianjinzi as a raw material, put it into a pulverizer for pulverization.

[0035] 2. Organic reagent extraction:

[0036] The stephenia powder was extracted with organic reagents, three consecutive extractions, each extraction time was 6h (heated to 60 degrees, and then heated for 6h). specific:

[0037] The first organic reagent extraction: add 2.5 kg of Stephania chinensis powder to 20 L of organic reagent, the organic reagent is ethyl acetate, stir well until the material liquid is uniform and there are no obvious lumps, turn on the water bath, extract for 6 hours, after the extraction is completed, collect the The supernatant was filtered with filter paper, and the supernatant was concentrated in a rotary evaporator and then transferred to a constant temperature blast drying oven at 60°C for drying to obtain the initial extract o...

Embodiment 2

[0043] Preparation of Diterpene Alcohol Esters (QJZ-6)

[0044] 1. Obtaining the primary extract of QJZ-6

[0045] 1. Crushing:

[0046] Take Qianjinzi as a raw material, put it into a pulverizer for pulverization.

[0047] 2. Organic reagent extraction:

[0048] The stephenia powder was extracted with organic reagents, three consecutive extractions, each extraction time was 6h (heated to 60 degrees, and then heated for 6h). specific:

[0049] The first organic reagent extraction: add 2.5 kg of Stephania chinensis powder to 20 L of organic reagent, the organic reagent is ethyl acetate, stir well until the material liquid is uniform and there are no obvious lumps, turn on the water bath, extract for 6 hours, after the extraction is completed, collect the The supernatant was filtered with filter paper, and the supernatant was concentrated in a rotary evaporator and then transferred to a constant temperature blast drying oven at 60°C for drying to obtain the initial extract of ...

Embodiment 3

[0056] Confirmation of QJZ-6 structure

[0057] 1. Purity analysis by HPLC:

[0058] The QJZ-6 component (Example 2) was completely dissolved with 50% n-hexane-ethanol solution, configured into a 5 mg / mL solution, and analyzed for purity by HPLC. YMC normal phase chromatographic column (250mm×4.6mm, 5μm, ), the detection wavelength is 210nm, the detection conditions are: the mobile phase is n-hexane and ethanol, 98% n-hexane, 2% ethanol isocratic elution for 30min, the flow rate is 0.6mL / min, the injection volume: 5μL, the temperature is 30°C, the High performance liquid phase detection purity reaches 99%, see HPLC spectrogram figure 1 .

[0059] 2. NMR analysis:

[0060] QJZ-6 was subjected to Bruker A.G AVI II 400PLUS, Hanmeng Biotechnology (Tianjin) Co., Ltd., and the NMR spectra were as follows figure 2 shown. The NMR data of QJZ-6 obtained from 1H NMR, 13C NMR, and HMBC spectra are shown in Table 1.

[0061] Table 1: 1H NMR (400MHz, J in Hz) and 13C NMR (100MHz) ...

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Abstract

The invention relates to a preparation method of a phorbol ester compound Euphorbia Factor L1. According to the method, a QJZ-6 original extract is all dissolved and separated with a preparation liquid phase normal-phase DAC (dynamic axial compression) chromatographic column, a binary mobile phase system is adopted for elution separation, a mobile phase A and a mobile phase B adopt combination of normal hexane and ethanol, the elution mode adopts gradient elution, the detection wavelength is 210 nm, and a target peak is collected and dried to obtain a target monomeric compound. The method has simple steps, good repeatability and high practicality and meets requirements for large-scale industrial production, and the purity of the separated and purified phorbol ester compound Euphorbia Factor L1 can be as high as 99%.

Description

technical field [0001] The invention relates to the field of compound production, in particular to a preparation method of a diterpene alcohol ester compound Qianjinzi No. 1. Background technique [0002] Qianjinzi is a poisonous traditional Chinese medicine that is rarely used. It mainly contains a large amount of fatty oil, and also contains compounds such as diterpenes, coumarins, and volatile oils. Modern research shows that diterpenoids are its main components and important active ingredients. Stephania contains L-factor (L-factor), a uniquely structured daughter terpene-type component. In addition to having many pharmacological activities, the multiple rings in its structure may further produce complex polymorphisms through cross-ring cyclization. ring structure. [0003] Malignant tumor is a serious disease with unknown cause. At present, surgery, radiotherapy, and chemotherapy are the main methods. Surgery is mostly suitable for early-stage cancer patients. Radiothe...

Claims

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Application Information

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IPC IPC(8): C07D303/32C07D301/32A61P35/00
CPCC07D301/32C07D303/32
Inventor 张耀洲杨珊珊顾朋嫒李聪聪
Owner TIANJIN LANGLI PHARMA CO LTD
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