CN104749123A - Method for determining content of polyphenol compound of cinnamic acid mother nucleus in sydney syrup - Google Patents
Method for determining content of polyphenol compound of cinnamic acid mother nucleus in sydney syrup Download PDFInfo
- Publication number
- CN104749123A CN104749123A CN201510160157.5A CN201510160157A CN104749123A CN 104749123 A CN104749123 A CN 104749123A CN 201510160157 A CN201510160157 A CN 201510160157A CN 104749123 A CN104749123 A CN 104749123A
- Authority
- CN
- China
- Prior art keywords
- solution
- snow pear
- reference substance
- chlorogenic acid
- sydney
- 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.)
- Pending
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for determining the content of polyphenol compound of cinnamic acid mother nucleus in sydney syrup. The method comprises the steps of preparing reference solution, preparing test solution, and determining by an ultraviolet and visible spectrophotometer, thereby determining the polyphenol compound of cinnamic acid mother nucleus, contained in 1g of sydney syrup, to be not less than 10.0mg as a qualified product through calculation by use of chlorogenic acid. Compared with the existing standard without content determination item, the method can control the inherent quality of a medicine by directly detecting the content of the polyphenol compound of the cinnamic acid mother nucleus; and besides, the determination method can be used for detecting conveniently and rapidly, has good stability and repeatability, and can well control the quality of the sydney syrup product.
Description
Technical field
The present invention relates to a kind of detection method of medicine, be specifically related to measure the method containing the polyphenolic substance content of the basic parent nucleus of derived from phenyl acrylic acid in snow pear paste.
Background technology
Snow pear paste is the Chinese medicine preparation that " the Sanitation Ministry medicine standard Traditional Chinese medicine historical preparation the tenth " records, there is clearing lung-heat heat, moisturize the effect of quenching the thirst, clinical conventional dry cough, chronic cough, because the former drug standards only define routine inspection, detect without assay item, effectively can not control the inherent quality of medicine, according to related request, need to revise and enlarge content measuring standard to said preparation, better to control product quality.
Snow pear paste is the soft extract that pears are made, bioactive ingredients for pears seldom studies have reported that, high performance liquid chromatography-tandem mass method is had to detect the research of polyphenol substance in pears in the recent period, detect tens of kinds of aldehydes matters, mainly contain chlorogenic acid, ursin, gallic acid, caffeic acid, coffee quininic acid, epicatechin, catechin, shaddock (skin) glycosides, rutin, Quercetin-glucoside, Quercetin-galactoside, quercetin-7-rhamnose glycosides, coumaric acid-glucoside, Quercetin-pentoside, rhamnose element-glucoside, Quercetin etc., polyphenolic substance has important biologically active, as anti-oxidant, Green Tea Extract, the functions such as anti-inflammatory.
Accordingly, the content measuring polyphenolic substance in snow pear paste is significant, chlorogenic acid is the polyphenolic substance containing the basic parent nucleus of derived from phenyl acrylic acid, this constituents has stronger characteristic ultraviolet absorption, with the content of this active component of determined by ultraviolet spectrophotometry, method is feasible, also better can reflect the quality of product.
Therefore, in the urgent need to researching and developing a kind of method measured containing the polyphenolic substance content of derived from phenyl acrylic acid parent nucleus in snow pear paste, the standard being used as evaluating snow pear paste quality has great importance.
Summary of the invention
For overcoming the deficiency of above-mentioned existing background technology, the object of the present invention is to provide a kind of method measured containing the polyphenolic substance content of derived from phenyl acrylic acid parent nucleus in snow pear paste product, to control the product quality of snow pear paste better.
The object of the invention is to be reached by following measure: a kind of method measured containing the polyphenolic substance content of derived from phenyl acrylic acid parent nucleus in snow pear paste, comprises the following steps:
(1) preparation of reference substance solution: get chlorogenic acid reference substance appropriate, accurately weighed, add ethanol and make the solution of every 1ml containing 10 μ g, obtain reference substance solution of chlorogenic acid;
(2) preparation of need testing solution: take snow pear paste 0.20g, puts 100ml volumetric flask, and the 5ml that adds water dissolves, and adds appropriate amount of ethanol, after ultrasonic process 20min, adds ethanol to scale, shakes up, with Filter paper filtering, get subsequent filtrate, obtain need testing solution;
(3) measure with ultraviolet-visible pectrophotometer: get reference substance solution and need testing solution respectively, measure absorbance at the wavelength place of 329nm, calculate, determine that the polyphenolic substance of the every 1g of snow pear paste containing derived from phenyl acrylic acid parent nucleus is with chlorogenic acid (C
16h
18o
9) meter, be no less than 10.0mg person for qualified.
Beneficial effect of the present invention is: the present invention uses ultraviolet spectrophotometry to measure the polyphenolic substance content containing derived from phenyl acrylic acid parent nucleus controlling snow pear paste product quality, compared in existing standard without the detection of assay item, the present invention directly can control the inherent quality of medicine by detecting the polyphenolic substance content containing derived from phenyl acrylic acid parent nucleus, and this assay method is easy to detect, rapid, stability and reproducible, can control the quality of snow pear paste product so better.
Accompanying drawing explanation
Fig. 1 is chlorogenic acid reference substance ultraviolet spectrogram;
Fig. 2 is test sample ultraviolet spectrogram;
Fig. 3 is negative control ultraviolet spectrogram;
Fig. 4 is chlorogenic acid canonical plotting.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in further detail, but they do not form limitation of the invention, only for example.Simultaneously by illustrating that advantage of the present invention will become clearly and easy understand.
Embodiment
The invention provides a kind of method measured containing the polyphenolic substance content of derived from phenyl acrylic acid parent nucleus in snow pear paste, comprise the following steps:
(1) preparation of reference substance solution: get chlorogenic acid reference substance appropriate, accurately weighed, add ethanol and make the solution of every 1ml containing 10 μ g, obtain reference substance solution of chlorogenic acid;
(2) preparation of need testing solution: take snow pear paste 0.20g, puts 100ml volumetric flask, and the 5ml that adds water dissolves, and adds appropriate amount of ethanol, after ultrasonic process 20min, adds ethanol to scale, shakes up, with Filter paper filtering, get subsequent filtrate, obtain need testing solution;
(3) measure with ultraviolet-visible pectrophotometer: get reference substance solution and need testing solution respectively, measure absorbance at the wavelength place of 329nm, calculate, determine that the polyphenolic substance of the every 1g of snow pear paste containing derived from phenyl acrylic acid parent nucleus is with chlorogenic acid (C
16h
18o
9) meter, be no less than 10.0mg person for qualified.
Correlation test is reported as follows:
1, instrument and reagent
Μ V-2501PC ultraviolet-visible pectrophotometer (Japanese Shimadzu), electronic balance (Beijing Sai Duolisi balance company limited), snow pear paste (Hubei is rectified pharmaceutcal corporation, Ltd and produced, lot number 130101,130102,130103); Chlorogenic acid reference substance (National Institute for Food and Drugs Control, lot number 110753-200413, for assay); Ethanol (Chemical Reagent Co., Ltd., Sinopharm Group), water are redistilled water.
The preparation of 1.1 reference substance solution
Get chlorogenic acid reference substance appropriate, accurately weighed, add ethanol and make the solution of every 1ml containing 10 μ g, obtain reference substance solution of chlorogenic acid;
The preparation of 1.2 reference substance stock solutions
Precision takes chlorogenic acid reference substance 2.82mg and is placed in 100ml volumetric flask, adds ethanol and is settled to scale, shake up, and obtains reference substance stock solution, and concentration is 28.2 μ g/ml.
The preparation of 1.3 need testing solutions
Take snow pear paste 0.20g, put 100ml volumetric flask, the 5ml that adds water dissolves, and adds appropriate amount of ethanol, after ultrasonic process 20min, adds ethanol to scale, shakes up, with Filter paper filtering, get subsequent filtrate, obtain need testing solution;
The preparation of 1.4 negative control solutions
The existing method for making of snow pear paste (" the Sanitation Ministry medicine standard Traditional Chinese medicine historical preparation the tenth "): get the chopping of fresh pears, squeeze the juice, the another device of pear juice is preserved; Pears slag boiling secondary is most to taste, collecting decoction, and filter, filtrate and pear juice merge, and are condensed into the clear cream that relative density is 1.33 ~ 1.38 (20 DEG C).Get the clear cream 1000g of pears, add water appropriate, boil, staticly settle, get supernatant and filter; Get granulated sugar 2000g and citric acid 3g, add water and boil in right amount, filter, add in above-mentioned filtrate, be concentrated into the relative density of regulation, obtain final product.
Make not containing the negative controls of pears by the above-mentioned method for making of snow pear paste, then make negative control solution by the method under " preparation of need testing solution " item.
2. method and result
2.1 determined wavelength are selected
Getting chlorogenic acid reference substance solution, snow pear paste need testing solution and negative control solution respectively, take ethanol as blank, and carry out 200 ~ 400nm length scanning uv-spectrogram in ultraviolet-visible spectrophotometer, its ultra-violet absorption spectrum is shown in Fig. 1 to Fig. 3.In Fig. 1, chlorogenic acid has absorption maximum crest at 329nm, is the characteristic absorption peak of the basic parent nucleus of cinnamic acid; In Fig. 2, test sample has maximum absorption band at about 280nm, and Fig. 3 negative control also presents larger absorption peak at 280nm, proves other material peak; Fig. 2 test sample has stronger absorption peak at about 329nm, and negative control at this wavelength without absorption peak, therefore can determine that determined wavelength is 329nm, measure the polyphenolic substance containing the basic parent nucleus of cinnamic acid.
2.2 typical curve
Get chlorogenic acid reference substance stock solution respectively, the serial solution that concentration is 28.2 μ g/ml, 14.1 μ g/ml, 9.87 μ g/ml, 7.05 μ g/ml, 3.525 μ g/ml is mixed with ethanol, take ethanol as blank, 329nm wavelength measures absorbance, with the concentration of reference substance solution for horizontal ordinate, absorbance is ordinate drawing standard curve, regression equation is: Y=0.0437x-4.3431, linear coefficient r=0.9998, show in 3.525 μ g/ml ~ 28.2 μ g/ml linear relationships good, the results are shown in Table 1 and Fig. 4.
Table 1 linear relationship
2.3 precision test
Get same reference substance solution, in 329nm wavelength place METHOD FOR CONTINUOUS DETERMINATION absorbance 5 times, precision the results are shown in Table 2, and to be 0.305, RSD be display mean light absorbency 0.23% shows that instrument precision is good, and this assay method is accurate, credible.
Table 2 Precision test result
2.4 replica test
Getting lot number is 130102 samples, prepares need testing solution by under test sample item, and parallel preparation 5 parts, measures its absorbance, and by regression equation calculation, the results are shown in Table 3, RSD is 0.98%, shows that the repeatability of the method is good.
Table 3 replica test result
2.5 stability test
Get with a need testing solution (lot number 130102), measure its absorbance respectively at 0h, 1h, 4h, 8h, 12h, 24h.Result RSD is 0.18%.Show that need testing solution is stable in 24h.The results are shown in Table 4.
Table 4 stability test result
2.6 average recovery
Get 5 parts, the snow pear paste sample (content is 6046.25 μ g/g) of known content, every part takes 0.20g snow pear paste sample, chlorogenic acid 1095 μ g is added respectively in each part, test solution is prepared by test sample method for making, measure its absorbance, calculate by regression equation, the results are shown in Table 5, chlorogenic acid application of sample average recovery rate is 95.59%.
Table 5 application of sample recovery test result
3. assay and limit are worked out
Prepare need testing solution to 3 batch samples, measure its absorbance by text condition, by regression equation calculation sample size, the results are shown in Table 6, the content of sample is with chlorogenic acid (C
16h
18o
9) count 11.55 (mg/g) to 12.09 (mg/g).
Table 6 snow pear paste sample size measurement result
Above-mentioned three batch samples are sample detection, are that full-page proof detects in actual production, and combine according to the content of 3 batch samples and produce reality, the every 1g of this product contains the polyphenolic substance of derived from phenyl acrylic acid parent nucleus with chlorogenic acid (C
16h
18o
9) must not count and be less than 10.0mg, determine that content is more than or equal to 10.0mg/g, illustrate that it is the certified products by existing snow pear paste method for making gained; If content is less than 10.0mg/g, illustrate that this snow pear paste is defective.
Conclusion: every data of above methodological study all meet the relevant regulations of quality standards in Chinese drugs research, method described in text is applicable to measure the polyphenolic substance content containing the basic parent nucleus of derived from phenyl acrylic acid in snow pear paste, therefore the inherent quality of snow pear paste medicine directly can be controlled by the content detecting above-mentioned polyphenolic substance, and this assay method is easy to detect, rapid, stability and reproducible, the method science, reasonable, feasible.Other unspecified part all belongs to prior art.
Claims (1)
1. measure the method containing the polyphenolic substance content of derived from phenyl acrylic acid parent nucleus in snow pear paste, it is characterized in that, comprise the following steps:
Step one: the preparation of reference substance solution: get chlorogenic acid reference substance appropriate, accurately weighed, add ethanol and make the solution of every 1ml containing 10 μ g, obtain reference substance solution of chlorogenic acid;
Step 2: the preparation of need testing solution: take snow pear paste 0.20g, puts 100ml volumetric flask, and the 5ml that adds water dissolves, and adds appropriate amount of ethanol, after ultrasonic process 20min, adds ethanol to scale, shakes up, with Filter paper filtering, get subsequent filtrate, obtain need testing solution;
Step 3: measure with ultraviolet-visible pectrophotometer: get reference substance solution and need testing solution respectively, absorbance is measured at the wavelength place of 329nm, calculate, determine that the polyphenolic substance of the every 1g of snow pear paste containing derived from phenyl acrylic acid parent nucleus is in chlorogenic acid, is no less than 10.0mg person for qualified.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510160157.5A CN104749123A (en) | 2015-04-07 | 2015-04-07 | Method for determining content of polyphenol compound of cinnamic acid mother nucleus in sydney syrup |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510160157.5A CN104749123A (en) | 2015-04-07 | 2015-04-07 | Method for determining content of polyphenol compound of cinnamic acid mother nucleus in sydney syrup |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104749123A true CN104749123A (en) | 2015-07-01 |
Family
ID=53589131
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510160157.5A Pending CN104749123A (en) | 2015-04-07 | 2015-04-07 | Method for determining content of polyphenol compound of cinnamic acid mother nucleus in sydney syrup |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104749123A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108872410A (en) * | 2018-03-22 | 2018-11-23 | 滨州医学院 | A kind of method for building up and its finger-print of lung-nourishing semifluid extract finger-print |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103645149A (en) * | 2013-12-11 | 2014-03-19 | 华中科技大学 | Method for synchronously detecting contents of total flavone and chlorogenic acid |
-
2015
- 2015-04-07 CN CN201510160157.5A patent/CN104749123A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103645149A (en) * | 2013-12-11 | 2014-03-19 | 华中科技大学 | Method for synchronously detecting contents of total flavone and chlorogenic acid |
Non-Patent Citations (5)
| Title |
|---|
| 尉芹等: "杜仲叶中绿原酸的提取工艺条件研究", 《林产化学与工业》 * |
| 康彬彬等: "超声波辅助乙醇提取栀子绿原酸的工艺研究", 《东南园艺》 * |
| 李燕婷等: "金银花中绿原酸的微波辅助提取工艺研究", 《化学与生物工程》 * |
| 苟占平等: "分光光度法测定5种1变种金银花中绿原酸含量", 《时珍国医国药》 * |
| 达超超等: "金银花中绿原酸提取工艺的研究", 《江西饲料》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108872410A (en) * | 2018-03-22 | 2018-11-23 | 滨州医学院 | A kind of method for building up and its finger-print of lung-nourishing semifluid extract finger-print |
| CN108872410B (en) * | 2018-03-22 | 2023-11-17 | 滨州医学院 | Method for establishing fingerprint spectrum of lung-moistening ointment and fingerprint spectrum thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103674638B (en) | A kind of method utilizing sense of taste finger printing quickly to differentiate the lycium barbarum productive year | |
| CN103940929B (en) | A kind of detection method for the treatment of the traditional Chinese medicine injection of cardiovascular and cerebrovascular disease | |
| CN102269751B (en) | Detection method of Liuweinengxiao preparation | |
| CN106018629B (en) | A kind of japanese fleeceflower leaf finger-print HPLC method and its application in the control of japanese fleeceflower leaf capsule quality | |
| CN110133148A (en) | A kind of hemp HPLC finger print measuring method | |
| CN110196290A (en) | Ellagic acid content assaying method in a kind of Rosa roxburghii Tratt | |
| CN109406645A (en) | A kind of Antisathmatic oral liquid for child epheday intermedia, the detection method for frying semen armeniacae amarae, Radix Glycyrrhizae, radix scutellariae | |
| Jin et al. | The association of dietary flavonoids, magnesium and their interactions with the metabolic syndrome in Chinese adults: a prospective cohort study | |
| Cui et al. | Determination of ginseng with different ages using a taste-sensing system | |
| CN105911154A (en) | Method for determination of chlorogenic acid, galuteolin and total flavone content of honeysuckle | |
| CN100437112C (en) | Method for inspecting Chinese medicinal preparation quality in treatment of old man eyes dieases | |
| CN102269752B (en) | Detection method for pharmaceutical composition preparation | |
| CN111537656B (en) | Identification method of tartary buckwheat extract | |
| CN104749123A (en) | Method for determining content of polyphenol compound of cinnamic acid mother nucleus in sydney syrup | |
| CN108653348A (en) | A kind of root of Dahurain angelica stem extraction Preparation Technology of Granules | |
| CN102175629A (en) | Biological activity detection-based evaluation method of quality of prepared radix rehmanniae | |
| CN104155383A (en) | Detection method of dandelion and viola philippica granules | |
| CN104007198A (en) | High performance liquid chromatography (HPLC) standard fingerprint spectrum of lucid ganoderma capsule preparation and construction method and application of standard fingerprint spectrum | |
| CN110823819A (en) | Compound radix polygoni multiflori preparata mulberry parasitic tea, preparation method and quality detection method | |
| CN112578055B (en) | Preparation process and quality control method of rhizoma Nelumbinis node and rhizoma Nelumbinis node charcoal control extract | |
| CN102288567B (en) | Method for detecting content of total flavone in Anweiyang capsule | |
| CN103091408B (en) | Method for determining content of hesperidin in Citrus Bioflavonoids | |
| CN104914186B (en) | The detection method of three kinds of compositions such as hard bar Leontopodium leontopodioides (Willd.) Beauv. or its processed product Content of Chlorogenic Acid | |
| CN102998272A (en) | Quality control method of mulberry particles | |
| CN104458954B (en) | A kind of dodder formulation granule finger printing and method for building up thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20150701 |
|
| RJ01 | Rejection of invention patent application after publication |