CN106053685A - SPE-HPLC method for determining content of phellodendrine in Leshu lotion - Google Patents
SPE-HPLC method for determining content of phellodendrine in Leshu lotion Download PDFInfo
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- CN106053685A CN106053685A CN201610503208.4A CN201610503208A CN106053685A CN 106053685 A CN106053685 A CN 106053685A CN 201610503208 A CN201610503208 A CN 201610503208A CN 106053685 A CN106053685 A CN 106053685A
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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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
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
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Abstract
The invention relates to a SPE-HPLC method for determining a content of phellodendrine in Leshu washing lotion. The method comprises the following steps of: A, preparing aliquid of a reference substance; B, preparing aliquid of a test sample: preparing the liquidof the test sample by adopting a solid phase extraction method; C, performing the liquid chromatographic detection; D, establishing a standard curve; and E, determining a sample. The testedliquid is prepared by selecting the solid phase extraction method, the extraction recovery rate about 100 percent can be obtained, inorganic salts and organic impurities in a test sample can be effectively removed, and the service life of a chromatographic column can be prolonged. The solid phase extraction method can process the sample in batches and is easy in automation, so that the working efficiency can be improved. A majority of methods reported by the existing literatures adopt a C18 chromatographic column, and the present method selects an amino column as an analysis column, so thatcompared with the C18 chromatographic column, the amino column has the advantages of high column efficiency, sharp peak pattern and little interference. The method is simple in operation, accurate in result, good in repeatability and less in impurity interference in the analysis process.
Description
Technical field
The present invention relates to phellodendrine content method in the happy washing liquid of relaxing of a kind of mensuration, measure in happy easypro washing liquid particularly to one
The SPE-HPLC method of phellodendrine content.
Background technology
Happy washing liquid of relaxing be Liuzhou city, Guangxi province healthcare hospital for women & children expert according to theory of Chinese medical science, make through clinical practice for many years
The Chinese medicine preparation (authentication code: osmanthus medicine word Z02060005) become, by the Radix Stemonae, Cortex Phellodendri, Radix Sophorae Flavescentis, Fructus Carpesii, Cortex Dictamni, Fructus Cnidii
Deng nine herbal medicine compositions, the clinical practice in more than 10 years shows, the reproductive tract infection such as gynecological's vulvitis, vaginitis are had by happy washing liquid of relaxing
Good curative effect, but said preparation lacks effective method of quality control always.
In recent years, Chinese medicine quality control method is conducted extensive research by analysis worker, establishes multiple thin layer chromatography
(TLC), high performance liquid chromatography (HPLC), high performance capillary electrophoresis etc. some composition in Chinese medicine gynecological lotion is carried out qualitative,
Quantitative analysis.Disclose following pertinent literature at present:
1, " the easypro liquid quality standard research of peace " of Liu Dongshun, Lu Wenquan, Piao Shujuan etc..
Chromatographic condition: ZORBAX SB-C18Post (4.6 mm × 250 mm, 5 μm) separates, column temperature 40 DEG C；With acetonitrile-
0.1% phosphoric acid (1000 mL add 50 μ L diethylamine) is eluent gradient eluting (0～8 min, 10%～18% acetonitrile；8～13
Min, 18%～30% acetonitrile；13～20 min, 30% acetonitrile), flow velocity 1.0mL/min, detect wavelength 284nm, sample size is 10 μ
L。
Need testing solution preparation method takes this product 10mL and is placed in conical flask, adds 20mL pure water, mixing, then enriching ammonia
Water 0.5mL, extracts 3 times (each 30mL) with dichloromethane, merges lower floor's extract, and 45 DEG C are evaporated, and dissolve with 5mL methanol and use
Initial flow is settled to 25mL mutually, filters, takes subsequent filtrate, to obtain final product.
Result: in 0. 05～2.5 μ g range, the peak area ratio of phellodendrine and concentration be good linear relationship (r=
0.9999), average recovery rate is respectively 101.62%, and precision RSD is 0.8%, and repeatability RSD is 0.4%.
Not enough: the relax pleasure of liquid and the court of peace relaxes the prescription of washing liquid and production technology is not quite similar, in preparation effective ingredient or
Impurity is the most different, and therefore the content assaying method of document report cannot be directly used to measure the phellodendrine of happy washing liquid of relaxing.Document
Need testing solution preparation method is liquid-liquid extraction method, the method complex operation, it is impossible to remove oil-soluble impurities.
2, Mao Guifu, Lu Xiaoyu etc. " in the happy washing liquid of relaxing of hplc simultaneous determination, phellodendrine and berberine contain
Amount ".
Chromatographic condition: chromatographic column is SPD-20AC18 post (4.6 mm × 250 mm, 5.0 μm)；Column temperature 30 DEG C；Flowing is mutually
Acetonitrile (A)-0.2% triethylamine (phosphoric acid adjusts PH 3.95) (B), gradient elution, elution program see table；Flow velocity 1.0 mL
min-1；Detection wavelength is 284 mn；Sample size is 20 μ L.
Table 1 gradient elution program
The preparation of need testing solution: relax ultrasonic 30 min of Wash Samples by pleasure, 0.45 μm filtering with microporous membrane takes its subsequent filtrate,
Obtain need testing solution.
Result: at 6.3～201.6 μ g mL-1In the range of, the peak area ratio of phellodendrine and concentration are good linear relationship
(r=0.9996), average recovery rate is respectively 100.6%, and precision RSD is 1.9%, and repeatability RSD is 1.9%.
Not enough: the author had previously set up the content assaying method of phellodendrine in happy washing liquid of relaxing and can be used for measuring the Huang of happy washing liquid of relaxing
Cypress alkali.But need testing solution preparation method is for directly measuring after filtering, and the method is simple to operate, but can not effectively remove fat-soluble
Impurity, understands impurity from chromatogram more, easy interference measurement, analyzes a small amount of sample rear pillar effect and is easy for making reduction.
In sum, due to the equal reason of Chinese medicine preparation complicated component, similar preparation recipe difference or production technology, respectively
Effective ingredient or the impurity of traditional Chinese medicine gynaecology lotion differ, and therefore discriminating and the content assaying method of document report can not be directly used as
The quality control method of happy washing liquid of relaxing, or method has certain defect, requires further improvement.
Summary of the invention
The technical problem to be solved in the present invention is: provides a kind of and measures the SPE-HPLC of phellodendrine content in happy washing liquid of relaxing
Method, the method is selected solid phase extraction to prepare need testing solution, can be obtained the recovery of extraction of nearly 100%, and effectively remove for examination
Inorganic salt in product solution and organic impurities, be conducive to extending chromatographic column service life, solid phase extraction can batch processing sample,
It is prone to automatization, improves work efficiency.This method is easy and simple to handle, and result is accurate, reproducible, impurity interference during analysis
Few.
The technical scheme solving above-mentioned technical problem is: a kind of measure the SPE-HPLC of phellodendrine content in happy washing liquid of relaxing
Method, comprises the following steps:
A, the preparation of reference substance solution: weigh phellodendrine reference substance, by methanol constant volume, make reference substance storing solution, by phellodendrine
Reference substance storing solution stepwise dilution, is prepared as series concentration reference substance working solution；
B, the preparation of need testing solution:
B1, easypro washing liquid supersound process of seeking pleasure, shake up, and filters, takes filtrate standby；
B2, take filtrate and cross the Bond Elut plexa PCX mixed type strong cation exchange pillar activated, use successively
0.5mol·L-1Hydrochloric acid, methanol and the washing of volumetric concentration 50% methanol solution, discard washing liquid, drain, finally molten with ammonia water-methanol
Liquid eluting, in ammonia water-methanol solution, ammonia is 2: 8 with the volume ratio of methanol, and coutroi velocity is at 1～1.5 mL min-1, take and wash
De-liquid is placed in air blow drying in 88～92 DEG C of water-baths, and the accurate flowing phase that adds, vortex concussion makes dissolved residue, obtains test sample molten
Liquid；
C, liquid chromatographic detection: after instrument state is stable, the reference substance working solution sample introduction prepared by step A, liquid chromatograph is examined
Surveying, on this basis, the need testing solution preparing step B carries out liquid chromatographic detection；
Liquid-phase chromatographic column selects Platisil-NH2Post, 5.0 μm, 250 mm × 4.6 mm；Testing conditions:
Column temperature: 30 DEG C；
Mensuration wavelength: 286 nm；
Sample size: 15 μ L or 20 μ L；
Flowing phase: 0.3% triethylamine-oxolane-acetonitrile solution, the wherein volume of 0.3% triethylamine, oxolane, acetonitrile
Ratio is 18: 12: 70, and 0.3% described triethylamine phosphoric acid adjusts pH value to be 3.82；
Flow velocity: 1.0 mL min-1；
D, the foundation of standard curve: with the sample introduction concentration of reference substance working solution as abscissa, peak area is vertical coordinate, draw standard
Curve；
E, sample determination: by the peak area of the phellodendrine of the need testing solution of mensuration, substitute into standard curve equation, be calculated confession
Phellodendrine content in test sample solution.
The further technical scheme of the present invention is: in step B1, and the condition of supersound process is power 400W, frequency 40kHz,
The time of supersound process is 25～35min.
In step B2, Bond Elut plexa PCX mixed type strong cation exchange pillar specification is 500mg/6mL, its
Activation is successively with 5 mL methanol, 0.5mol mL-1Hydrochloric acid solution 5mL rinses.
In step B2,0.5mol L-1Hydrochloric acid and methanol usage are respectively 10～15mL；The consumption of 50% methanol be 5～
7mL；The consumption of ammonia water-methanol solution is 18～25 mL.
In step D, the concentration of reference substance working solution is respectively 61.0 μ g mL-1、30.50μg·mL-1、15.25μg·mL-1。
Due to more containing Alumen in happy washing liquid of relaxing, directly its filtrate being carried out chromatography, inorganic salt easily separates out, and makes post
Effect reduces rapidly, and post pressure quickly raises, and result in blockage flow path system.Select solid phase extraction to prepare test liquid, can obtain near
The recovery of extraction of 100%, and effectively remove the inorganic salt in test sample and organic impurities, be conducive to extending chromatographic column and use the longevity
Life.Solid phase extraction can batch processing sample, it is easy to accomplish automatization, improves work efficiency.The method of existing document report is big
How all to use C18Chromatographic column, and this method selects nh 2 column to be analytical column, compares therewith, this method post effect height, peak type is sharp-pointed, dry
Disturb few.This method is easy and simple to handle, and result is accurate, reproducible, and during analysis, impurity interference is few.
The present invention uses the modern analysis means such as solid phase extraction, high performance liquid chromatography, sets up happy relaxing in lotion formulation
The quantitative analysis method of phellodendrine, provides the technical method of science, for setting up similar Chinese medicine preparation matter for improving said preparation quality
Prosecutor method provides reference frame.
Below, in conjunction with the accompanying drawings and embodiments a kind of of the present invention is measured the SPE-HPLC of phellodendrine content in happy washing liquid of relaxing
The technical characteristic of method is further described.
Accompanying drawing explanation
Fig. 1: the chromatogram of phellodendrine reference substance working solution.
The chromatogram of phellodendrine need testing solution prepared by Fig. 2: solid phase extraction method (the happy washing liquid lot number that relaxes:
2015121501).
The chromatogram of the negative sample solution of scarce Cortex Phellodendri prepared by Fig. 3: solid phase extraction method.
The chromatogram of phellodendrine need testing solution prepared by Fig. 4: solid phase extraction method (the happy washing liquid lot number that relaxes:
2016042001).
Fig. 5: the chromatogram of the phellodendrine need testing solution after filtering with microporous membrane.
In figure, 1 is phellodendrine.
Detailed description of the invention
1, instrument and reagent
Shimadzu LC-20AT quaternary gradient high performance liquid chromatographic system (LC-20AT pump, Rheodyne 7725i type injection valve, SPD-
20A UV-detector, CTO-20A column oven, the online degasser of DGu-20A, Japan's Shimadzu), (Shanghai is accurate for PHS-3C type PH meter
Scientific instrument company limited), KQ-300DB type numerical control ultrasonic cleaner (city of Kunshan has children outside the state plan Instrument Ltd.),
HANGPINGFA1004 type electronic balance (Shanghai balance equipment factory)；Agilent company Bond Elut Plexa PCX mixed type
Strong cation exchange pillar (500mg/6mL).
Phellodendrine reference substance (lot number: 110721, content >=98%, Wei Keqi bio tech ltd of Sichuan Province).First
Alcohol, acetonitrile are high-efficiency liquid chromatographic-grade reagent, and water is double distilled water, and other reagent are analytical pure.Happy Wash Samples (Liuzhou of relaxing
Healthcare hospital for women & children of city Drug Manufacturing Room, lot number: 2015121501,2015121502,2015121503,2016042001,
2016042002).
2, the preparation of reference substance solution
Precision weighs phellodendrine reference substance 6.10 mg and is placed in 10 mL volumetric flasks, adds methanol constant volume, obtains phellodendrine reference substance
Storing solution 0.61 mg mL-1.Take this reference substance storing solution the most respectively to be placed in right amount in 10 mL volumetric flasks, add methanol fixed
Hold, obtain concentration and be respectively 61.0 μ g mL-1、30.50μg·mL-1、15.25 μg·mL-1Phellodendrine reference substance working solution.
3, the preparation of need testing solution
Take happy washing liquid supersound process (power 400 W, the frequency 40kHz) 30min that relaxes of 500mL of sealing, shake up, filter, accurate amount
Take subsequent filtrate 2 mL, be added on Bond Elut plexa PCX mixed type strong cation exchange pillar (the most successively with methanol 5
mL、0.5mol·mL-1Hydrochloric acid solution 5mL activates) on, flow velocity the most per minute 1～1.5 mL, uses 0.5mol mL successively-1Salt
Acid solution 12mL, methanol 12 mL, 50% methanol aqueous solution 6mL washing, discard washing liquid, drain 1 min, then by 20mL ammonia-first
Alcoholic solution eluting (2: 8, volume ratio), collects eluent, takes 20mL eluent and is placed in 90 DEG C of water-baths and dries up, and residue precision adds
Flowing 2 mL vortex concussions mutually make dissolving, obtain need testing solution.
4, the preparation of negative sample solution
Separately weigh the medical material of scarce Cortex Phellodendri in the easypro washing liquid prescription ratio of pleasure, wash the feminine gender of the scarce Cortex Phellodendri of liquid preparing process preparation according to happy relaxing
Sample, then lack the negative sample solution of Cortex Phellodendri by method operation preparation under " 3, the preparation of need testing solution " item.
5, chromatographic condition
Chromatographic column: Platisil-NH2Post (250 mm × 4.6 mm, 5.0 μm)；Column temperature 30 DEG C；Flowing is 0.3% triethylamine mutually
(phosphoric acid adjusts PH 3.82)-oxolane-acetonitrile (18: 12: 70,V /V /V)；Flow velocity 1.0 mL min-1；Detection wavelength is
286 mn；Sample size is 15 or 20 μ L (standard curve sample size has 15 or 20 μ L, and remaining is 20 μ L).Theoretical cam curve is by Huang
Bai Jianfeng calculates should be not less than 12 000.
6, interference test
Measure negative sample solution, matrine reference substance solution and the confession of 2 lot numbers (2015121501,2016042001) respectively
The each 20 μ L of test sample solution detect, and result is shown in Fig. 1～Fig. 4.Happy washing liquid (lot number 2016042001) of relaxing after taking supersound process again
In right amount, with 0.45 μm filtering with microporous membrane, measuring subsequent filtrate 20 μ L sample detection, result is shown in Fig. 5.From chromatogram, negative
Sample solution is occurring without chromatographic peak on the matrine absworption peak position in the chromatogram of need testing solution, shows negative sample
In other impurity to measure noiseless.And test liquid prepared by filtering with microporous membrane, impurity peaks is the most, and severe jamming detects.
7, the foundation of standard curve
Measure 61.0,30.50,15.25 μ g mL-1Comparison liquid, respectively sample introduction 15 or 20 μ L, record peak area, with comparison
The sample introduction concentration of product working solution is abscissa, and peak area is vertical coordinate, draws standard curve.The recurrence side of phellodendrine standard curve
Cheng Wei: Y=32964 X+20251, r=0.9997.Result shows, phellodendrine is at 11.44～61.0 μ g mL-1In the range of linear
Relation is good.
8, precision test
Precision measures containing 30.50 μ g mL-1Phellodendrine comparison liquid sample introduction, is repeated 6 times.The RSD of phellodendrine is 0.94% (n=
6), show that instrument precision is good.
9, replica test
Precision measures same sample lots 6 parts, by legal system available test sample solution, sample introduction below " 3, the preparation of need testing solution " item
Measure content.As a result, the RSD of phellodendrine is respectively 1.63% (n=6), shows that the method repeatability is good.
10, stability test
Precision measures same need testing solution, and ambient temperatare is put, respectively at 0, and 2,4,6,8 h sample introductions, measure the face, peak of phellodendrine
Long-pending, the RSD calculating phellodendrine is 1. 93%, and result shows that need testing solution room temperature is stable in placing 8 h.
11, Solid-Phase Extraction recovery test
The concentration known phellodendrine reference substance solution of accurate measured amounts, by legal system below " 3, the preparation of need testing solution " item
Available test sample solution, measures the content of phellodendrine respectively, compares the calculating response rate with addition.Result see table.
The Solid-Phase Extraction recovery test result of table 2 phellodendrine (n =10)
12, average recovery
By sample ultrasonic 30 min of known phellodendrine content, filter paper filters, accurate draw 2 mL samples totally 9 parts be splined on respectively
Activation PCX mixed type strong cation exchange pillar in, be separately added into a certain amount of phellodendrine comparison liquid, according to " 3, test sample
The preparation of solution " method processes under item, and measure the content of phellodendrine and calculate the response rate.Result see table.
The average recovery result of the test (n=9) of table 3 phellodendrine
13, sample determination
Take 5 batches of pleasures to relax Wash Samples, prepare each need testing solution by method below " 3, the preparation of need testing solution " item, sample introduction respectively
Measure peak area, substitute into its content of standard curve Equation for Calculating.Result see table.
The measurement result (n=2) of phellodendrine content in the happy washing liquid of relaxing of table 4
。
Claims (5)
1. one kind measures the SPE-HPLC method of phellodendrine content in happy washing liquid of relaxing, it is characterised in that: comprise the following steps:
A, the preparation of reference substance solution: weigh phellodendrine reference substance, by methanol constant volume, make reference substance storing solution, by phellodendrine
Reference substance storing solution stepwise dilution, is prepared as series concentration reference substance working solution；
B, the preparation of need testing solution:
B1, easypro washing liquid supersound process of seeking pleasure, shake up, and filters, takes filtrate standby；
B2, take filtrate and cross the Bond Elut plexa PCX mixed type strong cation exchange pillar activated, use successively
0.5mol·L-1Hydrochloric acid, methanol and the washing of volumetric concentration 50% methanol solution, discard washing liquid, drain, finally molten with ammonia water-methanol
Liquid eluting, in ammonia water-methanol solution, ammonia is 2: 8 with the volume ratio of methanol, and coutroi velocity is at 1～1.5 mL min-1, take and wash
De-liquid is placed in air blow drying in 88～92 DEG C of water-baths, and the accurate flowing phase that adds, vortex concussion makes dissolved residue, obtains test sample molten
Liquid；
C, liquid chromatographic detection: after instrument state is stable, the reference substance working solution sample introduction prepared by step A, liquid chromatograph is examined
Surveying, on this basis, the need testing solution preparing step B carries out liquid chromatographic detection；
Liquid-phase chromatographic column selects Platisil-NH2Post, 5.0 μm, 250 mm × 4.6 mm；Testing conditions:
Column temperature: 30 DEG C；
Mensuration wavelength: 286 nm；
Sample size: 15 μ L or 20 μ L；
Flowing phase: 0.3% triethylamine-oxolane-acetonitrile solution, the wherein volume of 0.3% triethylamine, oxolane, acetonitrile
Ratio is 18: 12: 70, and 0.3% described triethylamine phosphoric acid adjusts pH value to be 3.82；
Flow velocity: 1.0 mL min-1；
D, the foundation of standard curve: with the sample introduction concentration of reference substance working solution as abscissa, peak area is vertical coordinate, draw standard
Curve；
E, sample determination: by the peak area of the phellodendrine of the need testing solution of mensuration, substitute into standard curve equation, be calculated confession
Phellodendrine content in test sample solution.
The most according to claim 1 a kind of measure the SPE-HPLC method of phellodendrine content in happy washing liquid of relaxing, it is characterised in that:
In step B1, the condition of supersound process is power 400W, frequency 40kHz, and the time of supersound process is 25～35min.
The most according to claim 1 a kind of measure the SPE-HPLC method of phellodendrine content in happy washing liquid of relaxing, it is characterised in that:
In step B2, Bond Elut plexa PCX mixed type strong cation exchange pillar specification is 500mg/6mL, and its activation is first
Afterwards with 5 mL methanol, 0.5mol mL-1Hydrochloric acid solution 5mL rinses.
The most according to claim 1 a kind of measure the SPE-HPLC method of phellodendrine content in happy washing liquid of relaxing, it is characterised in that:
In step B2,0.5mol L-1Hydrochloric acid and methanol usage are respectively 10～15mL；The consumption of 50% methanol is 5～7mL；Ammonia-first
The consumption of alcoholic solution is 18～25 mL.
The most according to claim 1 a kind of measure the SPE-HPLC method of phellodendrine content in happy washing liquid of relaxing, it is characterised in that:
In step D, the concentration of reference substance working solution is respectively 61.0 μ g mL-1、30.50μg·mL-1、15.25μg·mL-1。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108061761A (en) * | 2016-11-05 | 2018-05-22 | 天津天士力现代中药资源有限公司 | A kind of method for measuring alkaloid component content in blood-nourishing and brain-refreshing alcohol-extracted extract |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108061761A (en) * | 2016-11-05 | 2018-05-22 | 天津天士力现代中药资源有限公司 | A kind of method for measuring alkaloid component content in blood-nourishing and brain-refreshing alcohol-extracted extract |
| CN108061761B (en) * | 2016-11-05 | 2022-03-08 | 天津天士力现代中药资源有限公司 | Method for measuring content of alkaloid components in blood-nourishing brain-refreshing alcohol extract |
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