CN108362790A - A kind of construction method of Chinese patent drug " clear pancreas choleretic granules " HPLC characteristic spectrums - Google Patents
A kind of construction method of Chinese patent drug " clear pancreas choleretic granules " HPLC characteristic spectrums Download PDFInfo
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- CN108362790A CN108362790A CN201810075143.7A CN201810075143A CN108362790A CN 108362790 A CN108362790 A CN 108362790A CN 201810075143 A CN201810075143 A CN 201810075143A CN 108362790 A CN108362790 A CN 108362790A
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- 210000000496 pancreas Anatomy 0.000 title claims abstract description 59
- 239000000731 choleretic agent Substances 0.000 title claims abstract description 57
- 230000001989 choleretic effect Effects 0.000 title claims abstract description 57
- 239000008187 granular material Substances 0.000 title claims abstract description 57
- 238000001228 spectrum Methods 0.000 title claims abstract description 38
- 238000004128 high performance liquid chromatography Methods 0.000 title claims abstract description 31
- 238000010276 construction Methods 0.000 title claims abstract description 14
- 229940079593 drug Drugs 0.000 title claims abstract description 14
- 239000003814 drug Substances 0.000 title claims abstract description 14
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims abstract description 36
- YKRGDOXKVOZESV-WRJNSLSBSA-N Paeoniflorin Chemical compound C([C@]12[C@H]3O[C@]4(O)C[C@](O3)([C@]1(C[C@@H]42)O[C@H]1[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O1)O)C)OC(=O)C1=CC=CC=C1 YKRGDOXKVOZESV-WRJNSLSBSA-N 0.000 claims abstract description 35
- YKRGDOXKVOZESV-UHFFFAOYSA-N paeoniflorin Natural products O1C(C)(C2(CC34)OC5C(C(O)C(O)C(CO)O5)O)CC3(O)OC1C24COC(=O)C1=CC=CC=C1 YKRGDOXKVOZESV-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000012085 test solution Substances 0.000 claims abstract description 21
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000002360 preparation method Methods 0.000 claims abstract description 18
- 239000000243 solution Substances 0.000 claims abstract description 18
- 239000012088 reference solution Substances 0.000 claims abstract description 17
- 238000001514 detection method Methods 0.000 claims abstract description 11
- 238000010828 elution Methods 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 9
- 238000004811 liquid chromatography Methods 0.000 claims abstract description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 72
- 239000012071 phase Substances 0.000 claims description 50
- CWVRJTMFETXNAD-FWCWNIRPSA-N 3-O-Caffeoylquinic acid Natural products O[C@H]1[C@@H](O)C[C@@](O)(C(O)=O)C[C@H]1OC(=O)\C=C\C1=CC=C(O)C(O)=C1 CWVRJTMFETXNAD-FWCWNIRPSA-N 0.000 claims description 24
- PZIRUHCJZBGLDY-UHFFFAOYSA-N Caffeoylquinic acid Natural products CC(CCC(=O)C(C)C1C(=O)CC2C3CC(O)C4CC(O)CCC4(C)C3CCC12C)C(=O)O PZIRUHCJZBGLDY-UHFFFAOYSA-N 0.000 claims description 24
- CWVRJTMFETXNAD-KLZCAUPSSA-N Neochlorogenin-saeure Natural products O[C@H]1C[C@@](O)(C[C@@H](OC(=O)C=Cc2ccc(O)c(O)c2)[C@@H]1O)C(=O)O CWVRJTMFETXNAD-KLZCAUPSSA-N 0.000 claims description 24
- CWVRJTMFETXNAD-JUHZACGLSA-N chlorogenic acid Chemical compound O[C@@H]1[C@H](O)C[C@@](O)(C(O)=O)C[C@H]1OC(=O)\C=C\C1=CC=C(O)C(O)=C1 CWVRJTMFETXNAD-JUHZACGLSA-N 0.000 claims description 24
- 229940074393 chlorogenic acid Drugs 0.000 claims description 24
- FFQSDFBBSXGVKF-KHSQJDLVSA-N chlorogenic acid Natural products O[C@@H]1C[C@](O)(C[C@@H](CC(=O)C=Cc2ccc(O)c(O)c2)[C@@H]1O)C(=O)O FFQSDFBBSXGVKF-KHSQJDLVSA-N 0.000 claims description 24
- 235000001368 chlorogenic acid Nutrition 0.000 claims description 24
- BMRSEYFENKXDIS-KLZCAUPSSA-N cis-3-O-p-coumaroylquinic acid Natural products O[C@H]1C[C@@](O)(C[C@@H](OC(=O)C=Cc2ccc(O)cc2)[C@@H]1O)C(=O)O BMRSEYFENKXDIS-KLZCAUPSSA-N 0.000 claims description 24
- 239000013558 reference substance Substances 0.000 claims description 16
- 239000007788 liquid Substances 0.000 claims description 11
- 239000007791 liquid phase Substances 0.000 claims description 9
- 239000000706 filtrate Substances 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- 230000000694 effects Effects 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 2
- 230000002349 favourable effect Effects 0.000 abstract description 2
- 229940126680 traditional chinese medicines Drugs 0.000 abstract description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 8
- 238000004587 chromatography analysis Methods 0.000 description 7
- 230000014759 maintenance of location Effects 0.000 description 7
- 238000004458 analytical method Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 5
- 239000000047 product Substances 0.000 description 4
- 229910021642 ultra pure water Inorganic materials 0.000 description 4
- 239000012498 ultrapure water Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 241000205585 Aquilegia canadensis Species 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 241000218176 Corydalis Species 0.000 description 2
- 240000004980 Rheum officinale Species 0.000 description 2
- 235000008081 Rheum officinale Nutrition 0.000 description 2
- 235000021419 vinegar Nutrition 0.000 description 2
- 239000000052 vinegar Substances 0.000 description 2
- 235000003392 Curcuma domestica Nutrition 0.000 description 1
- 244000008991 Curcuma longa Species 0.000 description 1
- 241000237502 Ostreidae Species 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 230000002279 cholagogic effect Effects 0.000 description 1
- 235000003373 curcuma longa Nutrition 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- 235000020636 oyster Nutrition 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 230000003252 repetitive effect Effects 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 235000013976 turmeric Nutrition 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
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Abstract
A kind of construction method of Chinese patent drug " clear pancreas choleretic granules " HPLC characteristic spectrums, belongs to technical field of traditional Chinese medicines, this method includes：(1) preparation of test solution；(2) preparation of reference solution；(3) chromatographic condition：Chromatographic column is Agilent ZORBAX SB C18 (5 μm, 4.6 × 250mm) column, and mobile phase A is acetonitrile, and Mobile phase B is 0.2% phosphoric acid solution, and gradient elution, 0.9~1.1ml/min of flow velocity, 30~40 DEG C of column temperature, Detection wavelength is 235~245nm.Theoretical cam curve is calculated by Paeoniflorin peak should be not less than 3000.(4) it measures：According to high effective liquid chromatography for measuring characteristic spectrum.By establishing 10 batches of clear pancreas choleretic granules HPLC characteristic spectrums, it is determined that 10 characteristic peaks establish clear pancreas choleretic granules standard feature collection of illustrative plates.The present invention has the characteristics that convenient, fast, stable, precision is high, favorable reproducibility, can effectively control clear pancreas choleretic granules quality.
Description
Technical field
The invention belongs to technical field of traditional Chinese medicines, and in particular to the construction method of Chinese patent drug HPLC characteristic spectrums.
Background technology
Clear pancreas choleretic granules are (by oyster, turmeric, honeysuckle, radix bupleuri, rheum officinale, vinegar corydalis tuber, moutan bark, eight taste medicine of radix paeoniae rubra
Material forms.) standard records in the national drug standards, standard number：YBZ01052015.This product quality standard includes particle
Character；The thin layer of rheum officinale, honeysuckle and vinegar corydalis tuber differentiates；The assay of Paeoniflorin.Its quality standard only controls medicine simply
Method for qualitative and quantitative detection, it is difficult to whole comprehensive control product quality.
Invention content
The object of the present invention is to provide a kind of construction methods of Chinese patent drug " clear pancreas choleretic granules " HPLC characteristic spectrums.For
Quality control in clear pancreas choleretic granules production, overcomes the above-mentioned deficiency of the prior art,
The construction method of the clear pancreas choleretic granules HPLC characteristic spectrums of the present invention includes the following steps：
(1) preparation of test solution：Clear pancreas choleretic granules finely ground 0.5~1.5g of powder is taken, it is accurately weighed, it is placed in tool plug
In conical flask, 20~30ml of methanol is added in precision, and weighed weight is ultrasonically treated 20~40 minutes, lets cool, then weighed weight, uses
Methanol supplies the weight of less loss, shakes up, filtration, take subsequent filtrate to get.
(2) preparation of reference solution：Take Paeoniflorin, chlorogenic acid reference substance appropriate respectively, it is accurately weighed, add methanol to distinguish
Be made solution of every 1ml containing 100 μ g of Paeoniflorin, 50 μ g of chlorogenic acid to get.
(3) it measures：It is accurate respectively to draw reference solution and each 5~15 μ l of test solution, inject high performance liquid chromatography
Instrument, according to high effective liquid chromatography for measuring to get " clear pancreas choleretic granules " HPLC characteristic spectrums.
In preceding method, the chromatographic condition that the high performance liquid chromatography measures is：
Chromatographic column is Agilent ZORBAX SB-C18 (5 μm, 4.6 × 250mm) column, and mobile phase A is acetonitrile, Mobile phase B
For 0.2% phosphoric acid solution, gradient elution, 0.9~1.1ml/min of flow velocity, 30~40 DEG C of column temperature, Detection wavelength is 235~
245nm.Theoretical cam curve is calculated by Paeoniflorin peak should be not less than 3000.
Preferably, the construction method of a kind of Chinese patent drug " clear pancreas choleretic granules " HPLC characteristic spectrums, including it is following
Step：
(1) preparation of test solution：Clear pancreas choleretic granules finely ground powder 1.0g is taken, it is accurately weighed, it is placed in tool plug taper
In bottle, methanol 25ml is added in precision, and weighed weight is ultrasonically treated 30 minutes, lets cool, then weighed weight, less loss is supplied with methanol
Weight, shake up, filter, take subsequent filtrate to get.
(2) preparation of reference solution：Take Paeoniflorin, chlorogenic acid reference substance appropriate respectively, it is accurately weighed, add methanol to distinguish
Be made solution of every 1ml containing 100 μ g of Paeoniflorin, 50 μ g of chlorogenic acid to get.
(3) it measures：It is accurate respectively to draw reference solution and each 10 μ l of test solution, high performance liquid chromatograph is injected,
According to high effective liquid chromatography for measuring to get " clear pancreas choleretic granules " HPLC characteristic spectrums.
The chromatographic condition that the high performance liquid chromatography measures is preferably：
Chromatographic column is Agilent ZORBAX SB-C18 (5 μm, 4.6 × 250mm) column, and mobile phase A is acetonitrile, Mobile phase B
For 0.2% phosphoric acid solution, gradient elution, flow velocity 1.0ml/min, 35 DEG C of column temperature, Detection wavelength 240nm.Theoretical cam curve is pressed
Paeoniflorin peak, which calculates, should be not less than 3000.
During gradient elution, mobile phase A, the variation of the ratio of B are：0~10min, A phase 5%, B phases 95%；10~
15min, A phase 5%~10%, B phases 95%~90%；15~45min, A phase 10%~20%, B phases 90%~80%；45~
50min, A phase 20%~25%, B phases 80%~75%；50~60min, A phase 25%~30%, B phases 75%~70%；It is i.e. terraced
Spend elution program table：
The clear pancreas choleretic granules of 10 batches are established with the construction method of aforementioned one kind " clear pancreas choleretic granules " HPLC characteristic spectrums
HPLC characteristic spectrums, using Chinese Pharmacopoeia Commission《Similarity evaluation》2004A editions analyses, obtain
To the clear pancreas choleretic granules HPLC standard feature collection of illustrative plates being made of 10 characteristic peaks.Wherein No. 5 peak is chlorogenic acid peak, No. 6
Peak is Paeoniflorin peak.10 characteristic peaks are belonged to：1,2,6, No. 10 characteristic peaks are attributed to moutan bark medicinal material, 3,4, No. 5 spies
Sign peak is attributed to traditional Chinese medicine honeysuckle, and 6, No. 7 characteristic peaks are attributed to radix paeoniae rubra medicinal material, and 8, No. 9 characteristic peaks are attributed to Radix Bupleuri.
It is with reference to the peak peaks S, when calculating opposite reservation of each characteristic peak with the peaks S with Paeoniflorin peak in standard feature collection of illustrative plates
Between, within ± the 5% of specified value, the specified value is respectively the relative retention time：The peaks 0.11- 1, the peaks 0.18- 2,
The peaks 0.60- 3, the peaks 0.61- 4, the peaks 0.67- 5, the peaks 1.00- 6, the peaks 1.02- 7, the peaks 1.39- 8, the peaks 1.47- 9, the peaks 1.59- 10.
Clear pancreas choleretic granules sample is taken, is operated by above-mentioned same method, clear pancreas choleretic granules characteristic spectrum is obtained, using national medicine
The allusion quotation committee《Similarity evaluation》2004A editions to clear pancreas choleretic granules standard feature collection of illustrative plates and sample
Product characteristic spectrum is analyzed, and similarity is more than 0.90.
Advantageous effect：
1. the present invention establishes a kind of HPLC characteristic spectrum common patterns of Chinese patent drug " clear pancreas choleretic granules ", 10 have been demarcated
A characteristic peak, type and quantity of the characteristic spectrum than more comprehensively having reacted contained chemical composition of foundation avoid clear pancreas profit
The unicity and one-sidedness of courage granular mass control, are conducive to control product quality comprehensively.
2. present invention selection is measured at 240nm Detection wavelengths, appearance is more, and peak shape is good, is easy to differentiate, similitude
Height, stability is good, accurately and reliably.
3. the present invention has the characteristics that convenient, fast, stable, precision is high, favorable reproducibility, clear pancreas cholagogic can be effectively controlled
Granular mass.
Description of the drawings
Fig. 1 is the clear pancreas choleretic granules HPLC characteristic spectrums that the present invention measures；
Fig. 2 is the characteristic spectrum and common pattern of the clear pancreas choleretic granules of 10 batches；
Fig. 3 is the standard feature collection of illustrative plates of clear pancreas choleretic granules；
Specific implementation mode
The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention..
Embodiment 1：A kind of HPLC characteristic spectrum construction methods of clear pancreas choleretic granules
Instrument：1200 type high performance liquid chromatographs of Agilent, MS205DU type analysis balances
Reagent：Paeoniflorin reference substance, chlorogenic acid reference substance, liquid-phase chromatographic analysis with acetonitrile are chromatographically pure, remaining reagent is
Pure, water is analyzed to be provided by Fusong Chinese Medicine Co., Ltd. for ultra-pure water, clear pancreas choleretic granules.
The preparation of test solution：Clear pancreas choleretic granules fine powder 0.5g is taken, it is accurately weighed, it is placed in conical flask with cover, essence
Close addition methanol 20ml, weighed weight are ultrasonically treated 20 minutes, let cool, then weighed weight, the weight of less loss is supplied with methanol,
Shake up, filter, take subsequent filtrate to get.
The preparation of reference solution：Take Paeoniflorin, chlorogenic acid reference substance appropriate respectively, it is accurately weighed, add methanol to make respectively
At solution of every 1ml containing 100 μ g of Paeoniflorin, 50 μ g of chlorogenic acid to get.
It measures：Chromatographic condition：Chromatographic column is Agilent ZORBAX SB-C18 (5 μm, 4.6 × 250mm) column, mobile phase A
For acetonitrile, Mobile phase B is 0.2% phosphoric acid solution, gradient elution, flow velocity 0.9ml/min, 30 DEG C of column temperature, and Detection wavelength is
235nm.Theoretical cam curve is calculated by Paeoniflorin peak should be not less than 3000.The volume by volume concentration configuration of gradient elution program is as follows：
It is accurate respectively to draw reference solution and each 15 μ l of test solution, high performance liquid chromatograph is injected, according to efficient liquid
Phase chromatography measures to get " clear pancreas choleretic granules " HPLC characteristic spectrums.As shown in Figure 1.
Test sample characteristic spectrum is more than 0.90 with clear pancreas choleretic granules standard feature collection of illustrative plates similarity, is No. 6 peaks with reference to peak,
For Paeoniflorin peak；No. 5 peaks are chlorogenic acid peak.
Embodiment 2：A kind of HPLC characteristic spectrum construction methods of clear pancreas choleretic granules
Instrument：1200 type high performance liquid chromatographs of Agilent, MS205DU type analysis balances
Reagent：Paeoniflorin reference substance, chlorogenic acid reference substance, liquid-phase chromatographic analysis with acetonitrile are chromatographically pure, remaining reagent is
Pure, water is analyzed to be provided by Fusong Chinese Medicine Co., Ltd. for ultra-pure water, clear pancreas choleretic granules.
The preparation of test solution：Clear pancreas choleretic granules fine powder 1.5g is taken, it is accurately weighed, it is placed in conical flask with cover, essence
Close addition methanol 30ml, weighed weight are ultrasonically treated 40 minutes, let cool, then weighed weight, the weight of less loss is supplied with methanol,
Shake up, filter, take subsequent filtrate to get.
The preparation of reference solution：Take Paeoniflorin, chlorogenic acid reference substance appropriate respectively, it is accurately weighed, add methanol to make respectively
At solution of every 1ml containing 100 μ g of Paeoniflorin, 50 μ g of chlorogenic acid to get.
It measures：Chromatographic condition：Chromatographic column is Agilent ZORBAX SB-C18 (5 μm, 4.6 × 250mm) column, mobile phase A
For acetonitrile, Mobile phase B is 0.2% phosphoric acid solution, gradient elution, flow velocity 1.1ml/min, 40 DEG C of column temperature, and Detection wavelength is
245nm.Theoretical cam curve is calculated by Paeoniflorin peak should be not less than 3000.The volume by volume concentration configuration of gradient elution program is as follows：
It is accurate respectively to draw reference solution and each 5 μ l of test solution, high performance liquid chromatograph is injected, according to efficient liquid phase
Chromatography determination is to get " clear pancreas choleretic granules " HPLC characteristic spectrums.As shown in Figure 1.
Test sample characteristic spectrum is more than 0.90 with clear pancreas choleretic granules standard feature collection of illustrative plates similarity, is No. 6 peaks with reference to peak,
For Paeoniflorin peak；No. 5 peaks are chlorogenic acid peak.
Embodiment 3：A kind of HPLC characteristic spectrum construction methods of clear pancreas choleretic granules
Instrument：Wear peace U-3000 type high performance liquid chromatographs, MS205DU type analysis balances
Reagent：Paeoniflorin reference substance, chlorogenic acid reference substance, liquid-phase chromatographic analysis with acetonitrile are chromatographically pure, remaining reagent is
Pure, water is analyzed to be provided by Fusong Chinese Medicine Co., Ltd. for ultra-pure water, clear pancreas choleretic granules.
The preparation of test solution：Clear pancreas choleretic granules fine powder 1.0g is taken, it is accurately weighed, it is placed in conical flask with cover, essence
Close addition methanol 25ml, weighed weight are ultrasonically treated 30 minutes, let cool, then weighed weight, the weight of less loss is supplied with methanol,
Shake up, filter, take subsequent filtrate to get.
The preparation of reference solution：Take Paeoniflorin, chlorogenic acid reference substance appropriate respectively, it is accurately weighed, add methanol to make respectively
At solution of every 1ml containing 100 μ g of Paeoniflorin, 50 μ g of chlorogenic acid to get.
It measures：Chromatographic condition：Chromatographic column is Agilent ZORBAX SB-C18 (5 μm, 4.6 × 250mm) column, mobile phase A
For acetonitrile, Mobile phase B is 0.2% phosphoric acid solution, gradient elution, flow velocity 1.0ml/min, 35 DEG C of column temperature, and Detection wavelength is
240nm.Theoretical cam curve is calculated by Paeoniflorin peak should be not less than 3000.The volume by volume concentration configuration of gradient elution program is as follows：
It is accurate respectively to draw reference solution and each 10 μ l of test solution, high performance liquid chromatograph is injected, according to efficient liquid
Phase chromatography measures to get " clear pancreas choleretic granules " HPLC characteristic spectrums.As shown in Figure 1.
Test sample characteristic spectrum is more than 0.90 with clear pancreas choleretic granules standard feature collection of illustrative plates similarity, is No. 6 peaks with reference to peak,
For Paeoniflorin peak；No. 5 peaks are chlorogenic acid peak.
Embodiment 4：A kind of foundation of the HPLC standard feature collection of illustrative plates of clear pancreas choleretic granules
Instrument：Wear peace U-3000 type high performance liquid chromatographs, MS205DU type analysis balances
Reagent：Paeoniflorin reference substance, chlorogenic acid reference substance, liquid-phase chromatographic analysis with acetonitrile are chromatographically pure, remaining reagent is
Analyze that pure, water is ultra-pure water, (lot number is respectively clear pancreas choleretic granules：160101、160102、160103、161201、161202、
161203,170101 it, 170102,170103,171001) is provided by Fusong Chinese Medicine Co., Ltd..
The preparation of test solution：Clear pancreas choleretic granules fine powder 1.0g is taken, it is accurately weighed, it is placed in conical flask with cover, essence
Close addition methanol 25ml, weighed weight are ultrasonically treated 30 minutes, let cool, then weighed weight, the weight of less loss is supplied with methanol,
Shake up, filter, take subsequent filtrate to get.
The preparation of reference solution：Take Paeoniflorin, chlorogenic acid reference substance appropriate respectively, it is accurately weighed, add methanol to make respectively
At solution of every 1ml containing 100 μ g of Paeoniflorin, 50 μ g of chlorogenic acid to get.
Chromatographic condition：Chromatographic column is Agilent ZORBAX SB-C18 (5 μm, 4.6 × 250mm) column, and mobile phase A is second
Nitrile, Mobile phase B are 0.2% phosphoric acid solution, gradient elution, flow velocity 1.0ml/min, 35 DEG C of column temperature, Detection wavelength 240nm.Reason
3000 should be not less than by being calculated by Paeoniflorin peak by the number of plates.The volume by volume concentration configuration of gradient elution program is as follows：
It measures：It is accurate respectively to draw reference solution and each 10 μ l of test solution, high performance liquid chromatograph is injected, according to height
Effect liquid phase chromatogram method measures.
Methodological study
Precision test：It takes same a test solution continuous sample introduction 6 times, records chromatogram, the phase of more each characteristic peak
To retention time.As a result the RSD values of the relative retention time of all characteristic peaks are less than 3.0%, show that instrument precision is good.In detail
Thin result is as follows：
Repetitive test：It takes with a collection of (lot number：160101) clear 6 parts of pancreas choleretic granules are pressed test solution and are prepared respectively
Method prepares test solution, and sample introduction records chromatogram.As a result the RSD values of the relative retention time of all characteristic peaks are less than
3.0%, show that method repeatability is good.Detailed results are as follows：
Stability test：The test solution with a clear pancreas choleretic granules is taken, it is small 0,2,6,8,12,18,24 respectively
When sample introduction, record chromatogram.As a result the RSD values of the relative retention time of all characteristic peaks are less than 3.0%, show solution 24 hours
It has good stability.Detailed results are as follows：
Characteristic spectrum measures
The clear pancreas choleretic granules of 10 batches are measured using the above method, are recorded characteristic spectrum, are compared relative retention time,
As a result 10 batches of clear pancreas choleretic granules relative retention time RSD values are less than 3.0%, and detailed results are as follows：
Using Chinese Pharmacopoeia Commission《Similarity evaluation》
2004A editions analyses, characteristic spectrum and the common pattern for obtaining the clear pancreas choleretic granules of 10 batches are as shown in Figure 2.
Similarity calculation, 10 batches of clear pancreas choleretic granules characteristic spectrums and standard feature figure are carried out to 10 batches of clear pancreas choleretic granules characteristic spectrums
Spectrum similarity is all higher than 0.90.Detailed results are as follows：
The clear pancreas choleretic granules standard feature collection of illustrative plates established by the above method is as shown in Figure 3.
Claims (2)
1. a kind of construction method of Chinese patent drug " clear pancreas choleretic granules " HPLC characteristic spectrums, includes the following steps：
(1) preparation of test solution：Clear pancreas choleretic granules finely ground 0.5~1.5g of powder is taken, it is accurately weighed, it is placed in tool plug taper
In bottle, 20~30ml of methanol is added in precision, and weighed weight is ultrasonically treated 20~40 minutes, lets cool, then weighed weight, use methanol
The weight for supplying less loss, shakes up, filtration, take subsequent filtrate to get；
(2) preparation of reference solution：Take Paeoniflorin, chlorogenic acid reference substance appropriate respectively, it is accurately weighed, add methanol to be respectively prepared
Per solution of the 1ml containing 100 μ g of Paeoniflorin, 50 μ g of chlorogenic acid to get；
(3) it measures：It is accurate respectively to draw reference solution and each 5~15 μ l of test solution, high performance liquid chromatograph is injected, is shone
High effective liquid chromatography for measuring is to get " clear pancreas choleretic granules " HPLC characteristic spectrums；
In step (3), the chromatographic condition that the high performance liquid chromatography measures is：
Chromatographic column is Agilent ZORBAX SB-C18 (5 μm, 4.6 × 250mm) column, and mobile phase A is acetonitrile, and Mobile phase B is
0.2% phosphoric acid solution, gradient elution, mobile phase A, the variation of the ratio of B are：0~10min, A phase 5%, B phases 95%；10~
15min, A phase 5%~10%, B phases 95%~90%；15~45min, A phase 10%~20%, B phases 90%~80%；45~
50min, A phase 20%~25%, B phases 80%~75%；50~60min, A phase 25%~30%, B phases 75%~70%；Flow velocity
0.9~1.1ml/min, 30~40 DEG C of column temperature, Detection wavelength are 235~245nm.Theoretical cam curve should not by the calculating of Paeoniflorin peak
Less than 3000.
2. a kind of construction method of Chinese patent drug " clear pancreas choleretic granules " HPLC characteristic spectrums according to claim 1, most
Good construction method is as follows：
(1) preparation of test solution：Clear pancreas choleretic granules finely ground powder 1.0g is taken, it is accurately weighed, it is placed in conical flask with cover,
Methanol 25ml is added in precision, and weighed weight is ultrasonically treated 30 minutes, lets cool, then weighed weight, the weight of less loss is supplied with methanol
Amount, shake up, filter, take subsequent filtrate to get；
(2) preparation of reference solution：Take Paeoniflorin, chlorogenic acid reference substance appropriate respectively, it is accurately weighed, add methanol to be respectively prepared
Per solution of the 1ml containing 100 μ g of Paeoniflorin, 50 μ g of chlorogenic acid to get；
(3) it measures：It is accurate respectively to draw reference solution and each 10 μ l of test solution, high performance liquid chromatograph is injected, according to height
Effect liquid phase chromatogram method measures to get " clear pancreas choleretic granules " HPLC characteristic spectrums；
In step (3), the chromatographic condition that the high performance liquid chromatography measures is：
Chromatographic column is Agilent ZORBAX SB-C18 (5 μm, 4.6 × 250mm) column, and mobile phase A is acetonitrile, and Mobile phase B is
0.2% phosphoric acid solution, gradient elution, mobile phase A, the variation of the ratio of B are：0~10min, A phase 5%, B phases 95%；10~
15min, A phase 5%~10%, B phases 95%~90%；15~45min, A phase 10%~20%, B phases 90%~80%；45~
50min, A phase 20%~25%, B phases 80%~75%；50~60min, A phase 25%~30%, B phases 75%~70%；Flow velocity
1.0ml/min, 35 DEG C of column temperature, Detection wavelength 240nm.Theoretical cam curve is calculated by Paeoniflorin peak should be not less than 3000.
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| CN109839459A (en) * | 2019-02-22 | 2019-06-04 | 遵义医学院 | A kind of Radix Codonopsis multi-components content determination method based on the superposition of HPLC multi-wavelength |
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| CN112834672A (en) * | 2020-12-31 | 2021-05-25 | 四川新绿色药业科技发展有限公司 | Construction and detection method of rangooncreeper fruit formula particle characteristic spectrum |
| CN112834672B (en) * | 2020-12-31 | 2023-09-08 | 四川新绿色药业科技发展有限公司 | Construction and detection method of feature map of rangooncreeper fruit formula granule |
| CN115469028A (en) * | 2022-08-31 | 2022-12-13 | 修正药业集团股份有限公司 | HPLC (high performance liquid chromatography) characteristic spectrum construction method of Qinglin granules |
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