CN106053685B - A kind of SPE HPLC methods for determining golden cypress alkali content in happy easypro washing lotion - Google Patents

A kind of SPE HPLC methods for determining golden cypress alkali content in happy easypro washing lotion Download PDF

Info

Publication number
CN106053685B
CN106053685B CN201610503208.4A CN201610503208A CN106053685B CN 106053685 B CN106053685 B CN 106053685B CN 201610503208 A CN201610503208 A CN 201610503208A CN 106053685 B CN106053685 B CN 106053685B
Authority
CN
China
Prior art keywords
solution
easypro
washing lotion
happy
methanol
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201610503208.4A
Other languages
Chinese (zh)
Other versions
CN106053685A (en
Inventor
毛桂福
曾定元
王麟
杨妮
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Liuzhou Maternity and Child Healthcare Hospital
Original Assignee
Liuzhou Maternity and Child Healthcare Hospital
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Liuzhou Maternity and Child Healthcare Hospital filed Critical Liuzhou Maternity and Child Healthcare Hospital
Priority to CN201610503208.4A priority Critical patent/CN106053685B/en
Publication of CN106053685A publication Critical patent/CN106053685A/en
Application granted granted Critical
Publication of CN106053685B publication Critical patent/CN106053685B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • 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
    • 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
    • G01N2030/062—Preparation extracting sample from raw material

Abstract

The present invention relates to a kind of SPE HPLC methods for determining golden cypress alkali content in happy easypro washing lotion, comprise the following steps：A, the preparation of reference substance solution；B, the preparation of need testing solution：Need testing solution is prepared using solid phase extraction method；C, liquid chromatographic detection：D, the foundation of standard curve；E, sample determines.The present invention prepares test liquid from solid phase extraction, can obtain nearly 100% recovery of extraction, and effectively removes the inorganic salts and organic impurities in test sample, is advantageous to extend using life of chromatographic column.Solid phase extraction can batch processing sample, it is easy to accomplish automation, improves operating efficiency.The method of existing literature report all uses C mostly18Chromatographic column, and this method is analytical column from nh 2 column, is compared therewith, this method post effect is high, and peak type is sharp, and interference is few.This method is easy to operate, as a result accurately, reproducible, and impurity interference is few during analysis.

Description

A kind of SPE-HPLC methods for determining golden cypress alkali content in happy easypro washing lotion
Technical field
The present invention relates to phellodendrine content method in the happy easypro washing lotion of one kind measure, in more particularly to a kind of happy easypro washing lotion of measure The SPE-HPLC methods of golden cypress alkali content.
Background technology
Happy easypro washing lotion be Liuzhou city, Guangxi province healthcare hospital for women ＆ children expert according to theory of traditional Chinese medical science, made by clinical practice for many years Into Chinese medicine preparation (authentication code：Osmanthus medicine word Z02060005), by the tuber of stemona, golden cypress, kuh-seng, Lappula echinata, the root bark of shaggy-fruited dittany, frutus cnidii Formed Deng nine herbal medicines, the clinical practice in more than 10 years shows, happy easypro washing lotion has to RTIs such as gynaecology's vulvitis, vaginitis The effect of good, but said preparation lacks effective method of quality control always.
In recent years, analysis worker conducts extensive research to Chinese medicine quality control method, establishes a variety of thin-layered chromatography （TLC）, high performance liquid chromatography（HPLC）, capillary electrophoresis etc. some compositions in Chinese medicine gynecological lotion are carried out it is qualitative, Quantitative analysis.Following pertinent literature is disclosed at present：
1st, Liu Dongshun, Lu Wenquan, Piao Shujuan etc. " the easypro liquid quality standard research of peace ".
Chromatographic condition： ZORBAX SB-C18Post（4.6 mm × 250 mm, 5 μm）Separation, 40 DEG C of column temperature；With acetonitrile- 0.1% phosphoric acid（1000 mL add 50 μ L diethylamine）Eluted for eluent gradient（0~8 min, 10%~18% acetonitrile；8~13 Min, 18%~30% acetonitrile；13~20 min, 30% acetonitrile）, flow velocity 1.0mL/min, Detection wavelength 284nm, sample size is 10 μ L。
Need testing solution preparation method takes this product 10mL to be placed in conical flask, adds 20mL pure water, mixes, then enriching ammonia Water 0.5mL, extracted 3 times with dichloromethane（Each 30mL）, merge lower floor's extract, 45 DEG C are evaporated, and are dissolved and are used in combination with 5mL methanol Liquid phase is settled to 25mL, filtering, takes subsequent filtrate, produces.
As a result：In 0. 05~2.5 μ g ranges, peak area ratio and the concentration of phellodendrine are in good linear relationship（r = 0.9999）, average recovery rate is respectively 101.62%, precision RSD 0.8%, and repeated RSD is 0.4%.
Deficiency：The relax pleasure of liquid and the court of peace relaxes the prescription of washing lotion and production technology is not quite similar, in preparation active ingredient or Impurity is also different, therefore the content assaying method of document report cannot be directly used to the phellodendrine of the happy easypro washing lotion of measure.Document Need testing solution preparation method is liquid-liquid extraction method, and this method is cumbersome, it is impossible to removes oil-soluble impurities.
2nd, Mao Guifu, Lu Xiaoyu etc. " relax phellodendrine and jamaicin in washing lotion of hplc simultaneous determination pleasure contains Amount ".
Chromatographic condition：Chromatographic column is SPD-20AC18 posts (4.6 mm × 250 mm, 5.0 μm)；30 DEG C of column temperature；Mobile phase is The triethylamine of acetonitrile (A) -0.2% (phosphoric acid adjusts PH 3.95) (B), gradient elution, elution program see the table below；The mL of flow velocity 1.0 min-1；Detection wavelength is 284 mn；Sample size is 20 μ L.
The gradient elution program of table 1
The preparation of need testing solution：By happy easypro Wash Samples 30 min of ultrasound, 0.45 μm of filtering with microporous membrane, take it continuous Filtrate, produce need testing solution.
As a result：In 6.3~201.6 μ gmL-1In the range of, peak area ratio and the concentration of phellodendrine are in good linear relationship （r=0.9996）, average recovery rate is respectively 100.6%, precision RSD 1.9%, and repeated RSD is 1.9%.
Deficiency：The content assaying method that the author previously establishes phellodendrine in happy easypro washing lotion can be used for the Huang for determining happy easypro washing lotion Cypress alkali.But for need testing solution preparation method directly to be determined after filtering, this method is simple to operate, but can not effectively remove fat-soluble Impurity, understand that impurity is more from chromatogram, easy interference measurement, analyze a small amount of sample rear pillar effect and be easy for making reduction.
In summary, due to Chinese medicine preparation complicated component, similar preparation recipe is different or the reason such as production technology difference, respectively The active ingredient or impurity of traditional Chinese medicine gynaecology lotion differ, therefore the discriminating of document report and content assaying method can not be directly used as The quality control method of happy easypro washing lotion, or method have the defects of certain, it is necessary to further improve.
The content of the invention
The technical problem to be solved in the present invention is：A kind of SPE-HPLC for determining golden cypress alkali content in happy easypro washing lotion is provided Method, this method prepare need testing solution from solid phase extraction, can obtain nearly 100% recovery of extraction, and effectively remove for examination Inorganic salts and organic impurities in product solution, be advantageous to extend using life of chromatographic column, solid phase extraction can batch processing sample, It is easy to automate, improves operating efficiency.This method is easy to operate, as a result accurately, it is reproducible, during analysis impurity disturb It is few.
Solve above-mentioned technical problem technical scheme be：A kind of SPE-HPLC for determining golden cypress alkali content in happy easypro washing lotion Method, comprise the following steps：
A, the preparation of reference substance solution：Phellodendrine reference substance is weighed, with methanol constant volume, reference substance storing solution is made, by Huang Cypress alkali reference substance storing solution dilutes step by step, is prepared into series concentration reference substance working solution；
B, the preparation of need testing solution：
B1, easypro washing lotion of seeking pleasure are ultrasonically treated, and are shaken up, are filtered, take filtrate standby；
B2, filtrate is taken to be used successively after the Bond Elut plexa PCX mixed type strong cation exchange pillars activated 0.5mol·L-1Hydrochloric acid, methanol and the washing of the methanol solution of volumetric concentration 50%, discard washing lotion, drain, finally molten with ammonia water-methanol Liquid elutes, and the volume ratio of ammoniacal liquor and methanol is 2: 8 in ammonia water-methanol solution, and coutroi velocity is in 1~1.5 mLmin-1, take and wash De- liquid is placed in air blow drying in 88~92 DEG C of water-baths, and precision adds mobile phase, and vortex concussion makes dissolved residue, it is molten to produce test sample Liquid；
C, liquid chromatographic detection：After instrument state is stable, with the reference substance working solution sample introduction of step A preparations, liquid phase color Spectrum detection, on this basis, liquid chromatographic detection is carried out to need testing solution prepared by step B；
Liquid-phase chromatographic column selects Platisil-NH2Post, 5.0 μm, the mm of 250 mm × 4.6；Testing conditions：
Column temperature：30℃；
Determine wavelength：286 nm；
Sample size：15 μ L or 20 μ L；
Mobile phase：0.3% triethylamine-tetrahydrofuran-acetonitrile solution, wherein 0.3% triethylamine, tetrahydrofuran, acetonitrile Volume ratio is 18: 12: 70, and it is 3.82 that 0.3% described triethylamine phosphoric acid, which adjusts pH value,；
Flow velocity：1.0 mL·min-1；
D, the foundation of standard curve：Using the sample introduction concentration of reference substance working solution as abscissa, peak area is ordinate, is drawn Standard curve；
E, sample determines：By the peak area of the phellodendrine of the need testing solution of measure, calibration curve equation is substituted into, is calculated Golden cypress alkali content into need testing solution.
The present invention further technical scheme be：In step B1, 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 specifications are 500mg/6mL, its Activation is successively with 5 mL methanol, 0.5molmL-1Hydrochloric acid solution 5mL is rinsed.
In step B2,0.5molL-1Hydrochloric acid and methanol usage are respectively 10~15mL；The dosage of 50% methanol be 5~ 7mL；The dosage of ammonia water-methanol solution is 18~25 mL.
In step D, the concentration of reference substance working solution is respectively 61.0 μ gmL-1、30.50μg·mL-1、15.25μg·mL-1。
It is more due to containing alum in happy easypro washing lotion, chromatography directly is carried out to its filtrate, inorganic salts easily separate out, and make post Effect is rapid to be reduced, and the quick rise of post pressure, result in blockage flow path system.Test liquid is prepared from solid phase extraction, can be obtained near 100% recovery of extraction, and inorganic salts and organic impurities in test sample are effectively removed, be advantageous to extension chromatographic column and use the longevity Life.Solid phase extraction can batch processing sample, it is easy to accomplish automation, improves operating efficiency.The method of existing literature report is big All use C more18Chromatographic column, and this method is analytical column from nh 2 column, is compared therewith, this method post effect is high, and peak type is sharp, does Disturb few.This method is easy to operate, as a result accurately, reproducible, and impurity interference is few during analysis.
The present invention is established in happy easypro lotion formulation using modern analysis means such as solid phase extraction, high performance liquid chromatographies The quantitative analysis method of phellodendrine, to improve the technical method that said preparation quality provides science, to establish similar Chinese medicine preparation matter Prosecutor method provides reference frame.
Below, in conjunction with the accompanying drawings and embodiments to a kind of SPE-HPLC for determining golden cypress alkali content in happy easypro washing lotion of the present invention The technical characteristic of method is further described.
Brief description of the drawings
Fig. 1：The chromatogram of phellodendrine reference substance working solution.
Fig. 2：The chromatogram of phellodendrine need testing solution prepared by solid phase extraction method（Happy easypro washing lotion lot number： 2015121501）.
Fig. 3：The chromatogram of the negative sample solution of scarce golden cypress prepared by solid phase extraction method.
Fig. 4：The chromatogram of phellodendrine need testing solution prepared by solid phase extraction method（Happy easypro washing lotion lot number： 2016042001）.
Fig. 5：The chromatogram of phellodendrine need testing solution after filtering with microporous membrane.
1 is phellodendrine in figure.
Embodiment
1st, instrument and reagent
Shimadzu LC-20AT quaternary gradient high performances liquid chromatographic system (LC-20AT pumps, Rheodyne 7725i type sampling valves, SPD-20A UV-detectors, CTO-20A column ovens, DGu-20A on-line degassing machines, Japanese Shimadzu), PHS-3C types PH meters (Shanghai Precision scientific instrument Co., Ltd), KQ-300DB types numerical control ultrasonic cleaner (having children outside the state plan Instrument Ltd. in city of Kunshan), HANGPINGFA1004 types electronic balance (Shanghai balance equipment factory)；Agilent companies Bond Elut Plexa PCX mixed types 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 reagents are that analysis is pure.Happy easypro Wash Samples（Liuzhou Healthcare hospital for women ＆ children of city Drug Manufacturing Room, lot number：2015121501、2015121502、2015121503、2016042001、 2016042002）.
2nd, the preparation of reference substance solution
Precision weighs the mg of phellodendrine reference substance 6.10 and is placed in 10 mL volumetric flasks, adds methanol constant volume, produces phellodendrine pair According to the mgmL of product storing solution 0.61-1.Take the reference substance storing solution to be placed in right amount in 10 mL volumetric flasks respectively before use, add methanol Constant volume, it is respectively 61.0 μ gmL to obtain concentration-1、30.50μg·mL-1、15.25 μg·mL-1Phellodendrine reference substance work Liquid.
3rd, the preparation of need testing solution
Take the easypro washing lotion of 500mL pleasures of sealing to be ultrasonically treated (power 400 W, frequency 40kHz) 30min, shake up, filter, essence It is close to measure the mL of subsequent filtrate 2, it is added on Bond Elut plexa PCX mixed type strong cation exchange pillars and (uses methanol successively in advance 5 mL、0.5mol·mL-1Hydrochloric acid solution 5mL is activated) on, flow velocity 1~1.5 mL about per minute, 0.5molmL is used successively-1 Hydrochloric acid solution 12mL, the mL of methanol 12,50% methanol aqueous solution 6mL washings, discard washing lotion, drain 1 min, then with 20mL ammoniacal liquor- Methanol solution elutes（2: 8, volume ratio）, eluent is collected, takes 20mL eluents to be placed in 90 DEG C of water-baths and dries up, residue is accurate to be added Entering the mL vortex concussions of mobile phase 2 makes dissolving, produces need testing solution.
4th, the preparation of negative sample solution
The medicinal material of scarce golden cypress is separately weighed in the easypro washing lotion prescription ratio of pleasure, the scarce golden cypress of liquid preparing process preparation is washed according to happy relax Negative sample, then lack by method operation preparation under " 3, the preparation of need testing solution " item the negative sample solution of golden cypress.
5th, chromatographic condition
Chromatographic column：Platisil-NH2Post (250 mm × 4.6 mm, 5.0 μm)；30 DEG C of column temperature；Mobile phase is 0.3% 3 Ethamine (phosphoric acid adjusts PH 3.82)-tetrahydrofuran-acetonitrile（18: 12: 70,V/V/V）；The mLmin of flow velocity 1.0-1；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, which is calculated, should be not less than 12 000.
6th, interference test
Negative sample solution, matrine reference substance solution and 2 lot numbers are measured respectively（2015121501、2016042001） Each 20 μ L of need testing solution detected, as a result see Fig. 1~Fig. 4.Happy easypro washing lotion after being ultrasonically treated is taken again（Lot number 2016042001）In right amount, with 0.45 μm of filtering with microporous membrane, the μ L sample detections of subsequent filtrate 20 is measured, as a result see Fig. 5.From chromatogram To scheme visible, matrine of the negative sample solution in the chromatogram with need testing solution is absorbed on peak position to be occurred without chromatographic peak, Show that other impurities are noiseless to determining in negative sample.And test liquid prepared by filtering with microporous membrane, impurity peaks are especially more, sternly Weight Interference Detection.
7th, the foundation of standard curve
Measure 61.0,30.50,15.25 μ gmL-1Comparison liquid, respectively the μ L of sample introduction 15 or 20, record peak area, with right Sample introduction concentration according to product working solution is abscissa, and peak area is ordinate, draws standard curve.The recurrence of phellodendrine standard curve Equation is：The X+20251 of Y=32964, r=0.9997.As a result show, phellodendrine is in 11.44~61.0 μ gmL-1Scope interior lines Sexual intercourse is good.
8th, precision test
Precision is measured containing 30.50 μ gmL-1Phellodendrine comparison liquid sample introduction, is repeated 6 times.The RSD of phellodendrine is 0.94% (n =6), show that instrument precision is good.
9th, replica test
Precision measures same 6 parts of sample lots, by legal system available test sample solution below the preparation of need testing solution " 3, " item, Sample introduction determines content.As a result, the RSD of phellodendrine is respectively 1.63% (n=6), shows that this method repeatability is good.
10th, stability test
Precision measures same need testing solution, places at room temperature, respectively at 0,2,4,6,8 h sample introductions, determines phellodendrine Peak area, the RSD for calculating phellodendrine are 1. 93%, the results showed that need testing solution room temperature is placed stable in 8 h.
11st, SPE recovery test
The concentration known phellodendrine reference substance solution of accurate measured amounts, below the preparation of need testing solution " 3, " item Legal system available test sample solution, the content of phellodendrine, the calculating rate of recovery compared with addition are determined respectively.As a result see the table below.
The SPE recovery test result of the phellodendrine of table 2（n = 10）
12nd, average recovery
By the min of sample ultrasonic 30 of known golden cypress alkali content, filter paper filtration, precision draw 2 mL samples totally 9 parts respectively on Sample is separately added into a certain amount of phellodendrine comparison liquid in the PCX mixed type strong cation exchange pillars of activation, according to " 3, supply Method is handled under the preparation of test sample solution " item, is determined the content of phellodendrine and is calculated the rate of recovery.As a result see the table below.
The average recovery result of the test (n=9) of the phellodendrine of table 3
13rd, sample determines
Take 5 batches of pleasures to relax Wash Samples, prepares each need testing solution by method below the preparation of need testing solution " 3, " item, distinguish Sample introduction determines peak area, substitutes into calibration curve equation and calculates its content.As a result see the table below.
The measurement result (n=2) of golden cypress alkali content in the easypro washing lotion of the pleasure of table 4
。

Claims (5)

  1. A kind of 1. SPE-HPLC methods for determining golden cypress alkali content in happy easypro washing lotion, it is characterised in that：Comprise the following steps：
    A, the preparation of reference substance solution：Phellodendrine reference substance is weighed, with methanol constant volume, reference substance storing solution is made, by phellodendrine Reference substance storing solution dilutes step by step, is prepared into series concentration reference substance working solution；
    B, the preparation of need testing solution：
    B1, easypro washing lotion of seeking pleasure are ultrasonically treated, and are shaken up, are filtered, take filtrate standby；
    B2, filtrate is taken to be used successively after the Bond Elut plexa PCX mixed type strong cation exchange pillars activated 0.5mol·L-1Hydrochloric acid, methanol and the washing of the methanol solution of volumetric concentration 50%, discard washing lotion, drain, finally molten with ammonia water-methanol Liquid elutes, and the volume ratio of ammoniacal liquor and methanol is 2: 8 in ammonia water-methanol solution, and coutroi velocity is in 1~1.5 mLmin-1, take and wash De- liquid is placed in air blow drying in 88~92 DEG C of water-baths, and precision adds mobile phase, and vortex concussion makes dissolved residue, it is molten to produce test sample Liquid；
    C, liquid chromatographic detection：After instrument state is stable, with the reference substance working solution sample introduction of step A preparations, liquid chromatogram inspection Survey, on this basis, liquid chromatographic detection is carried out to need testing solution prepared by step B；
    Liquid-phase chromatographic column selects Platisil-NH2Post, 5.0 μm, the mm of 250 mm × 4.6；Testing conditions：
    Column temperature：30℃；
    Determine wavelength：286 nm；
    Sample size：15 μ L or 20 μ L；
    Mobile phase：0.3% triethylamine-tetrahydrofuran-acetonitrile solution, wherein the volume of 0.3% triethylamine, tetrahydrofuran, acetonitrile Than for 18: 12: 70, it is 3.82 that 0.3% described triethylamine phosphoric acid, which adjusts pH value,；
    Flow velocity：1.0 mL·min-1；
    D, the foundation of standard curve：Using the sample introduction concentration of reference substance working solution as abscissa, peak area is ordinate, draws standard Curve；
    E, sample determines：By the peak area of the phellodendrine of the need testing solution of measure, calibration curve equation is substituted into, confession is calculated Golden cypress alkali content in test sample solution.
  2. A kind of 2. SPE-HPLC methods for determining golden cypress alkali content in happy easypro washing lotion according to claim 1, it is characterised in that： In step B1, the condition of supersound process is power 400W, and frequency 40kHz, the time of supersound process is 25~35min.
  3. A kind of 3. SPE-HPLC methods for determining golden cypress alkali content in happy easypro washing lotion according to claim 1, it is characterised in that： In step B2, Bond Elut plexa PCX mixed type strong cation exchange pillar specifications are 500mg/6mL, and it is first that it, which is activated, Afterwards with 5 mL methanol, 0.5molmL-1Hydrochloric acid solution 5mL is rinsed.
  4. A kind of 4. SPE-HPLC methods for determining golden cypress alkali content in happy easypro washing lotion according to claim 1, it is characterised in that： In step B2,0.5molL-1Hydrochloric acid and methanol usage are respectively 10~15mL；The dosage of 50% methanol is 5~7mL；Ammoniacal liquor-first The dosage of alcoholic solution is 18~25 mL.
  5. A kind of 5. SPE-HPLC methods for determining golden cypress alkali content in happy easypro washing lotion according to claim 1, it is characterised in that： In step D, the concentration of reference substance working solution is respectively 61.0 μ gmL-1、30.50μg·mL-1、15.25μg·mL-1。
CN201610503208.4A 2016-06-27 2016-06-27 A kind of SPE HPLC methods for determining golden cypress alkali content in happy easypro washing lotion Active CN106053685B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610503208.4A CN106053685B (en) 2016-06-27 2016-06-27 A kind of SPE HPLC methods for determining golden cypress alkali content in happy easypro washing lotion

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610503208.4A CN106053685B (en) 2016-06-27 2016-06-27 A kind of SPE HPLC methods for determining golden cypress alkali content in happy easypro washing lotion

Publications (2)

Publication Number Publication Date
CN106053685A CN106053685A (en) 2016-10-26
CN106053685B true CN106053685B (en) 2018-03-27

Family

ID=57200502

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610503208.4A Active CN106053685B (en) 2016-06-27 2016-06-27 A kind of SPE HPLC methods for determining golden cypress alkali content in happy easypro washing lotion

Country Status (1)

Country Link
CN (1) CN106053685B (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103304562B (en) * 2013-07-04 2015-08-05 西南交通大学 The preparation method of a kind of Phellodendrine monomer and salt thereof
CN105548405A (en) * 2016-01-19 2016-05-04 李兴惠 Method for detecting traditional Chinese medicinal composition and preparation

Also Published As

Publication number Publication date
CN106053685A (en) 2016-10-26

Similar Documents

Publication Publication Date Title
CN111879887B (en) Radix astragali medicinal material and detection method and application of components in preparation thereof
CN102520079B (en) Method for rapidly measuring content of solanesol in tobaccos by using UPLC (Ultra Performance Liquid Chromatography)
CN104502518B (en) A kind of detection method for the treatment of the Chinese medicine preparation of baby anorexia
CN106124639A (en) The multicomponent content assaying method of Eucommia ulmoides
CN110780007B (en) Method for evaluating 6 component contents of mango cough relieving tablet by HPLC (high performance liquid chromatography) method
CN107315058A (en) A kind of method of total ginkgoic acid in detection ginkgo biloba succi
CN106324167B (en) Method for determining flavonoid components in astragalus extract by UPLC
CN104407082B (en) The detection method of alkylphenol compounds in a kind of ginkgo leaf raw material and preparation
CN109856270A (en) A method of with 7 index components in hplc simultaneous determination canopy powder granule
CN101791366A (en) Method for testing quality of Discorea nipponica Makino in different places and medicinal materials of same genera
CN106053685B (en) A kind of SPE HPLC methods for determining golden cypress alkali content in happy easypro washing lotion
CN101961405A (en) Method for testing content of pinoresinol diglucoside in compound eucommia bark tablet
CN104274727B (en) The quality determining method of clear battalion's oral liquid
CN108414667B (en) Method for detecting quality standard of Shengui Yixin granules
CN103623039A (en) Astragaloside extract product, preparing method therefor and quality standard control method therefor
CN106018642B (en) A kind of SPE HPLC methods for determining matrine content in happy easypro washing lotion
CN111579684B (en) Method for measuring content of total capsaicin in capsule wall material of capsule
CN102335333A (en) Method for detecting traditional Chinese medicine preparation of compound nutritions paste
CN112858550B (en) Method for analyzing similarity of ginkgo leaf medicines of different manufacturers and/or different batches of same manufacturers
CN107247106A (en) It is a kind of at the same determine Zhikening sucapsule in three kinds of active components method
CN109917045B (en) HPLC method for simultaneously measuring contents of 5 components in prepared rhizoma cibotii decoction pieces
CN110031533A (en) The method of polyphenols in Solid Phase Extraction and capillary electrophoresis technique combined separation detection mulberry leaf
CN106018577B (en) Three yellow party formulation ingredients detection methods and fingerprint map construction method
CN111965269A (en) Method for measuring oleanolic acid content and ursolic acid content in patrinia heterophylla by using ultra-high performance liquid chromatography
CN111175396A (en) Method for rapidly detecting six additives in food contact material by supercritical fluid chromatography

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant