CN109839463A - A kind of preparation of Cortex Moutan Dispersing Granules primary standard substance and method of quality control - Google Patents

Abstract

The invention discloses a kind of preparation of Cortex Moutan Dispersing Granules primary standard substance and method of quality control; using cortex moutan medicine materical crude slice as raw material; by water decoct twice, be concentrated under reduced pressure, Cortex Moutan Dispersing Granules primary standard substance is made in the process flows such as dry, global quality control is carried out using high performance liquid chromatography.The present invention is on the basis of motherland's Chinese Traditional Medicine decoction, in conjunction with modern times freeze-drying, diaphragm vacuum and low temperature concentration high technology equipment, pharmaceutical technology and high-efficient liquid phase chromatogram technology, and refer to cortex moutan chemical constitution study, the research of family's decocting process, the research of HPLC characteristic spectrum are carried out to cortex moutan, obtain a kind of reference substance that can be used as Cortex Moutan Dispersing Granules and arrange quality control.The substance can help to realize full constituents extraction, Manufacturing science, quality controllable, and cortex moutan Chinese medicinal granule and family that large-scale production may be implemented decoct the Appreciation gist of curative effect consistency, guarantee Chinese medicinal granule quality.The substance has preparation simply, and health is convenient for storage.

Description

A kind of preparation of Cortex Moutan Dispersing Granules primary standard substance and method of quality control

Technical field

The present invention relates to traditional Chinese medicine product technical field more particularly to a kind of preparations of Cortex Moutan Dispersing Granules primary standard substance And method of quality control.

Background technique

Cortex moutan, it is bitter in taste, pungent, slightly cold, there is the effect of clearing heat and cooling blood, activating microcirculation and removing stasis medicinal, enter ying blood, epidemic heat syndrome hair for heat Spot, hematemesis and epistaxis, night fever abating at dawn, lossless hectic fever due to yin, amenorrhea and algomenorrhea, the pain of injury caused by falling and tumbling, carbuncle sore tumefacting virus.

Cortex moutan is used as medicine with medicine materical crude slice, and the mode of decoction taken, The Quality of Sliced Herbal Medicine are unstable not before use Controllably, it decocts quality to be difficult to ensure, takes inconvenience, be not easy to store.And Chinese medicinal granule is to meet the excellent of concocted specification Matter medicinal material (prepared slices of Chinese crude drugs) is raw material, is extracted, is concentrated using modern high technology, product system class made of granulation, guaranteed original The nature and flavor feature of Chinese medicine.But how to guarantee quality of the Cortex Moutan Dispersing Granules in the case where losing medicine materical crude slice appearance character and with family Front yard decocts the consistency of curative effect, and there is presently no a reasonable controls, so the method that we imitate family's decoction, use are cold The method that the concentration of dry and diaphragm vacuum and low temperature is lyophilized prepares Cortex Moutan Dispersing Granules primary standard substance, is established with high performance liquid chromatography Its HPLC characteristic spectrum arranges the reference of quality control as Cortex Moutan Dispersing Granules.

Summary of the invention

The object of the invention is to remedy the disadvantages of known techniques, provides a kind of Cortex Moutan Dispersing Granules primary standard substance Preparation and method of quality control.

The present invention is achieved by the following technical solutions:

A kind of preparation method of Cortex Moutan Dispersing Granules primary standard substance, the preparation of the Cortex Moutan Dispersing Granules primary standard substance are adopted It is made with freeze-drying with the method that the concentration of diaphragm vacuum and low temperature combines.

The preparation method of the Cortex Moutan Dispersing Granules primary standard substance, specifically includes the following steps:

(1) cortex moutan medicine materical crude slice is weighed, first decocts the water for adding 8-10 times of medicine materical crude slice amount to measure, and first impregnates 30min, is cooked by slow fire again after boiling 30min filters to isolate decoction liquor while hot, and the second pan-fried plus 6-8 times amount water decocts 30min, filters, merging decoction liquor, mixing, Steam-volatile oil 2 hours, distillate is collected, it is spare；

(2) step 1 gained medical fluid is taken, vacuum degree -0.090-0.099 is adjusted, is concentrated into the clear of 1.07-1.09 at 65 DEG C or less Cream, it is spare；

(3) step 2 gained clear cream is placed in the stainless steel disc of certain specification, is placed in freeze drier, closed door-plate and open Refrigeration waits baffle temperature to be down to target temperature, transfers the program of formula access, opens vacuum pump, temperature control and formula and opens It closes, is freeze-dried, after freeze-drying, close vacuum pump, open vent valve, pump pressure reaches normal pressure, closes refrigeration, fast Speed opens door-plate, collects sample, sealing.

It is kept for 8 hours in the freezing dry process prior to -45 DEG C, is kept for 4 hours then at -30 DEG C, kept then at -10 DEG C It 3.5 hours, keeps then at 20 DEG C 3 hours, is finally kept for 30 hours in 50 DEG C.

The present invention also provides a kind of method of quality control of Cortex Moutan Dispersing Granules primary standard substance, and quality control is using high Effect liquid phase chromatogram method establishes the HPLC characteristic spectrum of Cortex Moutan Dispersing Granules primary standard substance.

The method of quality control, comprising the following steps:

(1) this product powder 0.2g is taken, it is accurately weighed respectively, it sets in 25ml measuring bottle, methanol 20ml, ultrasonic 30min is added, standing is put Cold, constant volume, filtering, filtrate is as test sample；

(2) Paeoniflorin 0.6mg is taken, is placed in 10ml volumetric flask, scale is dissolved and be settled to methanol, as object of reference；Take pellet Skin phenol 1.0mg, is placed in 10ml volumetric flask, scale is dissolved and be settled to methanol, as object of reference；

(3) it is tested using high performance liquid chromatography, it is accurate respectively to draw test solution, contrast solution 5-10 μ l, inject chromatography Instrument is measured according to following chromatographic condition:

Using octadecylsilane chemically bonded silica as filler；Mobile phase presses mobile phase binary gradient elutes:

Time (min)	Acetonitrile (%)	0.1% formic acid water (%)
			0	7	93
10	16	84
			10.01	17	83
30	20	80
			60	35	65
70	65	35
			80	80	20

Flow velocity: 1.0ml/min；Column temperature: 30 DEG C；Detection wavelength: 254nm；Number of theoretical plate should be not less than by the calculating of Paeonol peak 5000；

(4) by step 3 measurement result, analysis comparison is carried out, establishes the HPLC characteristic spectrum of Cortex Moutan Dispersing Granules primary standard substance.

The invention has the advantages that

High-tech is concentrated on the basis of motherland's Chinese Traditional Medicine decoction, in conjunction with modern times freeze-drying, diaphragm vacuum and low temperature in the present invention Skill equipment, pharmaceutical technology and high-efficient liquid phase chromatogram technology, and cortex moutan chemical constitution study is referred to, family is carried out to cortex moutan and is decocted Technical study, the research of HPLC characteristic spectrum are boiled, a kind of reference that can be used as Cortex Moutan Dispersing Granules and arrange quality control is obtained Substance.The substance can help to realize full constituents extraction, Manufacturing science, quality controllable, and the tree peony of large-scale production may be implemented Skin Chinese medicinal granule and family decoct the Appreciation gist of curative effect consistency, guarantee Chinese medicinal granule quality.The substance has Preparation is simple, and health is convenient for storage.

Detailed description of the invention

Fig. 1 show Cortex Moutan Dispersing Granules primary standard substance HPLC characteristic spectrum.

Specific embodiment

Below in conjunction with specific example, technical scheme is described further:

Embodiment 1

The preparation of cortex moutan primary standard substance granule:

(1) raw material is weighed: cortex moutan medicine materical crude slice 3400g；

(2) cortex moutan medicine materical crude slice is put into cooking pot for herbs, decocted twice, added 9 times of medicine materical crude slice amount of water for the first time, impregnate 30 minutes, decoct 30 minutes, second plus 7 times of water of medicine materical crude slice amount, decoct 30 minutes, and medical fluid filtration, filtrate merges, and steam-volatile oil 2 is small When, distillate is collected, it is spare；Medical fluid is pumped into concentration tank, is concentrated (vacuum degree -0.090-0.099MPa), is concentrated into relatively close Degree be 1.07-1.09(65 DEG C) clear cream, it is spare；

(3) step 2 gained clear cream is placed in the stainless steel disc of certain specification, is placed in freeze drier, closed door-plate and open Refrigeration waits baffle temperature to be down to target temperature.The program of formula access is transferred, vacuum pump, temperature control and formula is opened and opens It closes, is freeze-dried, concrete operations are shown in Table 1:

The design of 1 lyophilisation condition of table

Segment number	Target temperature DEG C	Hour	Minute	Control
					1	-45	8	0	0
2	-30	4	0	30
					3	-10	3	30	10
4	20	3	0	10
					5	50	30	0	10

Freeze-drying terminates, and closes vacuum pump, opens vent valve, and pump pressure reaches normal pressure, closes refrigeration, opens door-plate rapidly, receives Collect sample, sealing；

(4) step 3 gained dried cream powder is crushed, crosses 80 meshes；It is first packed with 10 grams of polyethylene, then packed with 50 grams of full aluminium bags (50g/ bags of loading amount) is to get finished product.

Embodiment 2

The method of quality control of Cortex Moutan Dispersing Granules primary standard substance HPLC characteristic spectrum:

(1) this product powder, medicinal powder, medicine materical crude slice powder 0.2g are taken, it is accurately weighed respectively, it sets in 25ml measuring bottle, methanol is added 20ml, ultrasonic 30min, standing are let cool, constant volume, and filtering, filtrate is as test sample；

(2) Paeoniflorin 0.6mg is taken, is placed in 10ml volumetric flask, scale is dissolved and be settled to methanol, as object of reference；Take pellet Skin phenol 1.0mg, is placed in 10ml volumetric flask, scale is dissolved and be settled to methanol, as object of reference；

(3) accurate respectively to draw for examination referring to four 0512 high performance liquid chromatography of the general rule tests of " Chinese Pharmacopoeia " version in 2015 Product solution, contrast solution 5-10 μ l, injecting chromatograph are measured according to following chromatographic condition；

Using octadecylsilane chemically bonded silica as filler；Mobile phase presses mobile phase binary gradient elutes (such as table 2)；Flow velocity: 1.0ml/min；Column temperature: 30 DEG C；Detection wavelength: 254nm；Number of theoretical plate is calculated by Paeonol peak should be not less than 5000；

2 mobile phase elution requirement of table

Time (min)	Acetonitrile (%)	0.1% formic acid water (%)
			0	7	93
10	16	84
			10.01	17	83
30	20	80
			60	35	65
70	65	35
			80	80	20

(4) by step 3 measurement result, carry out analysis comparison, with the HPLC characteristic spectrum of Cortex Moutan Dispersing Granules primary standard substance into Row control.

As shown in Figure 1, showing to contain cortex moutan ingredient in test sample.

Embodiment 3

Moisture, extract and assay measurement in Cortex Moutan Dispersing Granules primary standard substance:

To moisture, extract and assay in the Cortex Moutan Dispersing Granules primary standard substance of 3 batches prepared in aforementioned manners It is detected.Moisture is detected according to a conventional method.Determination of extractives is according to the hot dipping under ethanol soluble extractives measuring method item (four general rules 2201 of " Chinese Pharmacopoeia " version in 2015) measurement, uses ethanol as solvent.Assay is according to (" Chinese Pharmacopoeia " 2015 Year version one) measuring method under cortex moutan item.Every inspection result is as shown in table 3, shows that indices comply with standard.

The every testing result of table 3

Lot number	Moisture (%)	Extract (%)	Paeonol content (%)
				1	4.5	65.53	3.22
2	4.7	63.41	3.00
				3	4.2	60.80	4.04

Claims (5)

1. a kind of preparation method of Cortex Moutan Dispersing Granules primary standard substance, which is characterized in that the Cortex Moutan Dispersing Granules benchmark The preparation of substance is made using freeze-drying with the method that the concentration of diaphragm vacuum and low temperature combines.

2. the preparation method of Cortex Moutan Dispersing Granules primary standard substance according to claim 1, which is characterized in that specifically include Following steps:

(1) cortex moutan medicine materical crude slice is weighed, first decocts the water for adding 8-10 times of medicine materical crude slice amount to measure, and first impregnates 30min, is cooked by slow fire again after boiling 30min filters to isolate decoction liquor while hot, and the second pan-fried plus 6-8 times amount water decocts 30min, filters, merging decoction liquor, mixing, Steam-volatile oil 2 hours, distillate is collected, it is spare；

(2) step 1 gained medical fluid is taken, vacuum degree -0.090-0.099 is adjusted, is concentrated into the clear of 1.07-1.09 at 65 DEG C or less Cream, it is spare；

(3) step 2 gained clear cream is placed in the stainless steel disc of certain specification, is placed in freeze drier, closed door-plate and open Refrigeration waits baffle temperature to be down to target temperature, transfers the program of formula access, opens vacuum pump, temperature control and formula and opens It closes, is freeze-dried, after freeze-drying, close vacuum pump, open vent valve, pump pressure reaches normal pressure, closes refrigeration, fast Speed opens door-plate, collects sample, sealing.

3. according to claim 1 or the preparation method of 2 described in any item Cortex Moutan Dispersing Granules primary standard substances, feature exist In, it is kept for 8 hours in the freezing dry process prior to -45 DEG C, is kept for 4 hours then at -30 DEG C, it is small then at -10 DEG C of holdings 3.5 When, it keeps then at 20 DEG C 3 hours, is finally kept for 30 hours in 50 DEG C.

4. a kind of method of quality control of Cortex Moutan Dispersing Granules primary standard substance, which is characterized in that quality control uses efficient liquid Phase chromatography establishes the HPLC characteristic spectrum of Cortex Moutan Dispersing Granules primary standard substance.

5. method of quality control according to claim 4, which comprises the following steps:

(1) this product powder 0.2g is taken, it is accurately weighed respectively, it sets in 25ml measuring bottle, methanol 20ml, ultrasonic 30min is added, standing is put Cold, constant volume, filtering, filtrate is as test sample；

(2) Paeoniflorin 0.6mg is taken, is placed in 10ml volumetric flask, scale is dissolved and be settled to methanol, as object of reference；Take pellet Skin phenol 1.0mg, is placed in 10ml volumetric flask, scale is dissolved and be settled to methanol, as object of reference；

(3) it is tested using high performance liquid chromatography, it is accurate respectively to draw test solution, contrast solution 5-10 μ l, inject chromatography Instrument is measured according to following chromatographic condition:

Using octadecylsilane chemically bonded silica as filler；Mobile phase presses mobile phase binary gradient elutes:

Time (min) Acetonitrile (%) 0.1% formic acid water (%) 0 7 93 10 16 84 10.01 17 83 30 20 80 60 35 65 70 65 35 80 80 20

Flow velocity: 1.0ml/min；Column temperature: 30 DEG C；Detection wavelength: 254nm；Number of theoretical plate should be not less than by the calculating of Paeonol peak 5000；

(4) by step 3 measurement result, analysis comparison is carried out, establishes the HPLC characteristic spectrum of Cortex Moutan Dispersing Granules primary standard substance.