CN105372378A - Quality inspection method of cortex moutan dispersing granules - Google Patents
Quality inspection method of cortex moutan dispersing granules Download PDFInfo
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- CN105372378A CN105372378A CN201410429349.7A CN201410429349A CN105372378A CN 105372378 A CN105372378 A CN 105372378A CN 201410429349 A CN201410429349 A CN 201410429349A CN 105372378 A CN105372378 A CN 105372378A
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Abstract
Provided is a quality inspection method of cortex moutan dispersing granules. The method comprises a thin-layer chromatography identification method and a content determination method. The thin-layer chromatography identification method is adopted to conduct qualitative identification on the cortex moutan dispersing granules, and meanwhile a high-performance liquid chromatography method is adopted to conduct content determination on paeonol in the cortex moutan dispersing granules. The quality inspection method of the cortex moutan dispersing granules is established, and the product quality is effectively controlled.
Description
Technical field
The present invention relates to a kind of TLC Identification and content assaying method of Cortex Moutan Dispersing Granules, belong to traditional Chinese medicine quality detection field.
Background technology
Cortex Moutan Dispersing Granules is the granule that the dry root skin of ranunculaceae peony PaeoniasuffruticosaAndr is made, gas fragrance, mildly bitter flavor and puckery, there is clearing heat and cooling blood, the effect such as promoting blood circulation and removing blood stasis, is mainly used in: heat enters ying blood, febrile virulent maculae, hematemesis and epistaxis, night fever abating at dawn, lossless hectic fever due to yin, through closing dysmenorrhoea, fall and flutter the pain of injury, carbuncle sore tumefacting virus.
Chinese medicinal granule is the single medicinal material medicine materical crude slice meeting concocted specification is raw material, adopt advanced technologies and the method for modern pharmaceutical industry, through extracting, concentrated, dry, make the manufactured goods of certain specification for medical institutions' clinical formulation, it is a kind of supplementary form of the prepared slices of Chinese crude drugs, can substitute the prepared slices of Chinese crude drugs for clinician, the large bag medicine materical crude slice marmite becoming traditional Chinese medicine decoction closes to be decocted, filters that drink-service etc. is numerous and diversely operating as large productions of standardization industry, inner wrapping, water rush and namely takes.Compared with traditional Chinese medicine medicine materical crude slice, the Chinese medicinal granule of industrialized mass production, quality is more homogeneous, result (data and the collection of illustrative plates) favorable reproducibility detected according to quality standard, both the property of medicine of the former prepared slices of Chinese crude drugs, flavour of a drug and drug effect had been maintained, have again do not need decoct, determined curative effect, use, easy to carry, the advantages such as safety, being the product that traditional Chinese medicine medicine materical crude slice grows with each passing hour, is the modern Chinese herbal medicine decoction of " coming from medicine materical crude slice, higher than medicine materical crude slice ".Chinese medicinal granule, not only for tcm clinical practice formula, also can be used as the aspect such as raw material medicine, health food, food, daily cosmetics, fine chemical product, veterinary medicine of Chinese patent drug.It will become a new industry between the prepared slices of Chinese crude drugs and Chinese patent drug.
Compared with traditional Chinese herbs decoction, the advantages such as Chinese medicinal granule has exempts to decoct easy clothes, easily stores, easy to carry.But Chinese medicinal granule has lost the resemblance of medicinal material after the processing of series of processes, be difficult to differentiate to identify medicinal material by proterties, and also different with crude drug in its quality control.Thin-layered chromatography is simple to operate, convenient, is applicable to the Qualitive test of Chinese crude drug and various Chinese medicine preparation.High performance liquid chromatography is highly sensitive, is applicable to the quantitative test of various preparation.The present invention adopts thin-layered chromatography to carry out Qualitive test to Cortex Moutan Dispersing Granules, adopt high performance liquid chromatography to carry out assay to Paeonol wherein simultaneously, be intended to the quality determining method setting up a kind of Cortex Moutan Dispersing Granules, the method can be used for the quality control of Cortex Moutan Dispersing Granules, to ensureing that the stability of product quality and the validity of clinical application and security are significant.
Summary of the invention
The object of the present invention is to provide the quality determining method of Cortex Moutan Dispersing Granules, the method comprises: (1) TLC Identification assay method and (2) high performance liquid chromatography content assaying method.Wherein:
(1) TLC distinguish: get this product powder 1g, add diethyl ether 10ml, close plug, jolting 10 minutes, filter, filtrate volatilizes, and residue adds acetone 2ml makes dissolving, as need testing solution; Separately get moutan bark control medicinal material 0.5g, add diethyl ether 10ml, close plug, jolting 10 minutes, and filter, filtrate volatilizes, and residue adds acetone 2ml makes dissolving.Get Paeonol reference substance again, add acetone and make the solution of every 1ml containing 5mg, product solution in contrast; Thin-layered chromatography according to Chinese Pharmacopoeia version in a 2010 annex VIB is tested, draw each 10 μ l of above-mentioned solution, put respectively on same silica gel g thin-layer plate, with thiacyclohexane-ethyl acetate (3:1) for developping agent, launch, take out, dry, spray with the acid 5% ferric trichloride ethanolic solution of hydrochloric acid, it is clear that hot blast blows to spot development.In test sample chromatogram, on the position corresponding to reference substance chromatogram and control medicinal material chromatogram, aobvious identical blue brown spot.
(2) assay: measure according to high performance liquid chromatography (Chinese Pharmacopoeia version in 2010 annex VID);
Chromatographic condition: take octadecylsilane chemically bonded silica as filling agent; With tetrahydrofuran-4% phosphate aqueous solution (70:30) for mobile phase; DAD detecting device detects, and determined wavelength is 274nm, column temperature 30 DEG C, flow velocity: 1ml/min.
The preparation of reference substance solution: it is appropriate that precision takes Paeonol reference substance, adds methyl alcohol and makes the solution of every 1ml containing 0.5mg, to obtain final product.
The preparation of need testing solution: get Cortex Moutan Dispersing Granules powder 0.4g, accurately weighed, put in 10ml measuring bottle, add methyl alcohol appropriate, sonic oscillation 30 minutes, puts to room temperature, adds methyl alcohol to scale, filters, and discard just filtrate, getting subsequent filtrate is need testing solution.
Determination method: accurate absorption reference substance solution 10 μ l, need testing solution 10 μ l respectively, injection liquid chromatography, measures, to obtain final product.
The method that the invention has the advantages that is simple, accurate, highly sensitive, precision, good stability, HPLC method is adopted to measure the content of Paeonol in Cortex Moutan Dispersing Granules, peak shape is good, degree of separation is high, can be used as the quality control of Cortex Moutan Dispersing Granules and investigates the effective technology means of technology stability, being significant to improving the quality of products.
Accompanying drawing explanation
Fig. 1: Cortex Moutan Dispersing Granules TLC schemes, and 1 is Paeonol reference substance; 2 is control medicinal materials; 3 ~ 8 is six batches of Cortex Moutan Dispersing Granules test samples.
Fig. 2: Cortex Moutan Dispersing Granules HPLC collection of illustrative plates, A is reference substance collection of illustrative plates; B is test sample 1 Paeonol.
Embodiment
Embodiment 1: the indentification by TLC of Cortex Moutan Dispersing Granules
TLC distinguish: get this product powder 1g, add diethyl ether 10ml, close plug, jolting 10 minutes, filter, filtrate volatilizes, and residue adds acetone 2ml makes dissolving, as need testing solution; Separately get moutan bark control medicinal material 0.5g, add diethyl ether 10ml, close plug, jolting 10 minutes, and filter, filtrate volatilizes, and residue adds acetone 2ml makes dissolving.Get Paeonol reference substance again, add acetone and make the solution of every 1ml containing 5mg, product solution in contrast; Thin-layered chromatography according to Chinese Pharmacopoeia version in a 2010 annex VIB is tested, draw each 10 μ l of above-mentioned solution, put respectively on same silica gel g thin-layer plate, with thiacyclohexane-ethyl acetate (3:1) for developping agent, launch, take out, dry, spray with the acid 5% ferric trichloride ethanolic solution of hydrochloric acid, it is clear that hot blast blows to spot development.In test sample chromatogram, on the position corresponding to reference substance chromatogram and control medicinal material chromatogram, aobvious identical blue brown spot.
Embodiment 2: the content assaying method of Cortex Moutan Dispersing Granules
Assay: measure according to high performance liquid chromatography (Chinese Pharmacopoeia version in 2010 annex VID);
1, instrument and reagent
(1) instrument: DioexUltiMate3000 high performance liquid chromatograph, DAD detecting device, quaternary gradient pump, chameleon data handling system.
(2) reagent: tetrahydrofuran, methyl alcohol are chromatographically pure reagent (FisherScientific), and water is distilled water, it is pure that other reagent is analysis.Paeonol reference substance (lot number: 110708-200506) is purchased from Nat'l Pharmaceutical & Biological Products Control Institute.
2, experiment condition
(1) chromatographic condition: chromatographic column: UnitaryC185um100A (4.6mm × 150mm); Mobile phase: tetrahydrofuran-4% phosphate aqueous solution (70:30); Determined wavelength is 274nm; Column temperature: 30 DEG C; Flow velocity: 1.0mL/min.
3, methodological study
(1) investigation of the range of linearity:
Precision measures Paeonol reference substance solution 1.5,2.0,3.0 μ l and reference substance storing solution 1.0,5.0,10.0 μ l, injection liquid chromatography carries out chromatographic determination, measures peak area by above-mentioned chromatographic condition, and with peak area (Y), linear regression is carried out to sample size (X), obtain typical curve.
Obtain regression equation: Y=17.8017x-1.4441, r=0.99982; Show that Paeonol is linear within the scope of 0.5008 ~ 12.52 μ g.
The results are shown in Table 1.
Table 1 Paeonol reference substance measurement result
(2) precision test: the accurate reference substance solution 5 μ l that draws repeats sample introduction 6 times, records integrating peak areas value RSD < 2%, the results are shown in Table 2.
Table 2 Precision test result
(3) stability test: get same test sample (lot number: 120915) solution 10 μ l, 5 times are measured by method under assay item, RSD (n=5) < 2% of result Paeonol integrating peak areas value, shows in 8 hours stable.The results are shown in Table 3.
Table 3 stability test result
(4) replica test: by the content assaying method drafted, to same batch sample (lot number: 120915) make 5 parts of test liquids respectively, record Paeonol peak area and calculate content, RSD < 2%, the results are shown in Table 4.
Table 4 sample repeatability test (n=2)
(5) test with yield: the sample (lot number 120915) getting known content, precision adds a certain amount of Paeonol reference substance respectively, by test sample preparation and assay method, parallelly does 6 groups, the results are shown in Table 5.
Table 5 Paeonol determination of recovery rates result
(6) sample determination:
Get Cortex Moutan Dispersing Granules and be about 0.4g, accurately weighed, put in 10ml measuring bottle, add methyl alcohol appropriate, sonic oscillation 30 minutes, puts to room temperature, adds methyl alcohol to scale, filters, and discard just filtrate, getting subsequent filtrate is need testing solution; Accurate absorption reference substance solution 10 μ l respectively, each 10 μ l of sample test liquid, measure by above-mentioned chromatographic condition, the results are shown in Table 6.
Table 6 sample size measurement result (n=2)
Claims (3)
1. a detection method for Cortex Moutan Dispersing Granules, the method comprises:
(1) TLC Identification, and
(2) high performance liquid chromatography content assaying method.
2. the detection method of Cortex Moutan Dispersing Granules described in claim 1, wherein said TLC Identification is: (1) need testing solution is prepared: get Cortex Moutan Dispersing Granules powder 1g, add diethyl ether 10ml, close plug, jolting 10 minutes, filter, filtrate volatilizes, residue adds acetone 2ml makes dissolving, as need testing solution; (2) reference substance solution preparation: separately get moutan bark control medicinal material 0.5g, add diethyl ether 10ml, close plug, jolting 10 minutes, filter, filtrate volatilizes, and residue adds acetone 2ml makes dissolving; Get Paeonol reference substance again, add acetone and make the solution of every 1ml containing 5mg, product solution in contrast; (3) determination method: according to the thin-layered chromatography test of Chinese Pharmacopoeia version in a 2010 annex VIB, draw each 10 μ l of above-mentioned solution, put respectively on same silica gel g thin-layer plate, with thiacyclohexane-ethyl acetate (3:1) for developping agent, launch, take out, dry, spray with the acid 5% ferric trichloride ethanolic solution of hydrochloric acid, it is clear that hot blast blows to spot development; In test sample chromatogram, on the position corresponding to reference substance chromatogram and control medicinal material chromatogram, aobvious identical blue brown spot.
3. the quality determining method of Cortex Moutan Dispersing Granules described in claim 1, wherein said high performance liquid chromatography content assaying method is: (1) chromatographic condition: take octadecylsilane chemically bonded silica as filling agent; Tetrahydrofuran-4% phosphate aqueous solution (70:30) is mobile phase; DAD detecting device detects, determined wavelength: 274nm; Column temperature 30 DEG C, flow velocity: 1ml/min; (2) preparation of reference substance solution, it is appropriate that precision takes Paeonol reference substance, adds methyl alcohol and make the solution of every 1ml containing 0.5mg, to obtain final product; (3) preparation of need testing solution: get Cortex Moutan Dispersing Granules powder 0.4g, accurately weighed, put in 10ml measuring bottle, add methyl alcohol appropriate, sonic oscillation 30 minutes, puts to room temperature, adds methyl alcohol to scale, filter, discard just filtrate, getting subsequent filtrate is need testing solution; (4) determination method: accurate absorption reference substance solution 10 μ l, need testing solution 10 μ l respectively, injection liquid chromatography, measures, to obtain final product.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113917041A (en) * | 2021-11-01 | 2022-01-11 | 湖南新汇制药股份有限公司 | Quality detection method for standard decoction of moutan bark |
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| KR20060084083A (en) * | 2005-01-17 | 2006-07-24 | 경북대학교 산학협력단 | Methods for increasing paeonol content in moutan cortex, and the method for extraction of paeonol having increased contents obtained by the method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113917041A (en) * | 2021-11-01 | 2022-01-11 | 湖南新汇制药股份有限公司 | Quality detection method for standard decoction of moutan bark |
| CN113917041B (en) * | 2021-11-01 | 2024-03-15 | 湖南新汇制药股份有限公司 | Quality detection method for cortex moutan standard decoction |
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Application publication date: 20160302 |