CN107782830A - The content assaying method of Isopsoralen in a kind of oteoporosis treating medicinal capsule - Google Patents
The content assaying method of Isopsoralen in a kind of oteoporosis treating medicinal capsule Download PDFInfo
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- CN107782830A CN107782830A CN201610721302.7A CN201610721302A CN107782830A CN 107782830 A CN107782830 A CN 107782830A CN 201610721302 A CN201610721302 A CN 201610721302A CN 107782830 A CN107782830 A CN 107782830A
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- methanol
- isopsoralen
- water
- oteoporosis
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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
- G01N30/62—Detectors specially adapted therefor
- G01N30/74—Optical detectors
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Abstract
The content assaying method of Isopsoralen in a kind of oteoporosis treating medicinal capsule, precision weigh Isopsoralen 171mg, put in 25mL measuring bottles, add methanol to dissolve and are diluted to scale, shake up and produce and (contain Isopsoralen 0.0684mg per 1mL).Oteoporosis treating medicinal capsule content 50mg is taken, it is accurately weighed, addition methanol 25mL in conical flask with cover is put, weighed weight, 20min is ultrasonically treated, lets cool, then weighed weight, less loss weight is supplied with methanol, is shaken up.Filtered with miillpore filter, take subsequent filtrate to produce.Chromatographic condition, methanol-water (V methanol: V water=48: 52)；Flow velocity 11mL/min；40 DEG C of column temperature；Wavelength 245nm.Assay method, it is accurate respectively to draw μ L of reference substance solution 1, the μ L of need testing solution 15, liquid chromatograph is injected, measure, produces result.
Description
Technical field
The present invention relates to a kind of content assaying method of Isopsoralen in oteoporosis treating medicinal capsule, specifically with a kind of bone
Dredge the content assaying method of Isopsoralen in curing capsule.
Background technology
The compound preparation that currently known oteoporosis treating medicinal capsule is made up of kinds of traditional Chinese medicines such as barrenwort, psoralea corylifolia, the fruit of glossy privets,
There is certain curative effect to climacteric women osteoporosis.Psoralea corylifolia is one of monarch drug in a prescription in side, its main component be psoralen with
Isopsoralen.
The content of the invention
Research object：Instrument and reagent；High performance liquid chromatograph (LC10AT infusion pumps, SPD10A UV-detectors, Japan
Shimadzu)；Isopsoralen reference substance (Nat'l Pharmaceutical ＆ Biological Products Control Institute)；Methanol (chromatographically pure)；Remaining reagent is analysis
It is pure.Method and result；The preparation of reference substance solution, precision weigh Isopsoralen reference substance 171mg, put in 25mL measuring bottles, add
Methanol dissolves and is diluted to scale, shakes up, and produces and (contains Isopsoralen 00684mg per 1mL).The preparation of need testing solution, takes
Oteoporosis treating medicinal capsule content 50mg, it is accurately weighed, put in conical flask with cover, precision adds methanol 25mL, weighed weight, at ultrasound
20min is managed, is let cool, then weighed weight, less loss weight is supplied with methanol, is shaken up.Filtered with miillpore filter, take subsequent filtrate to produce.
Chromatographic condition, chromatographic column：EMerck Lichroshpher 100RP18(250mm×4mm,5μm)；Mobile phase：Methanol-water (V first
Alcohol: V water=48: 52)；Flow velocity 11mL/min；40 DEG C of column temperature；Wavelength 245nm.Assay method, accurate absorption reference substance is molten respectively
μ L of liquid 1, the μ L of need testing solution 15, liquid chromatograph is injected, measure, produces result.The drafting of standard curve, precision draw control
The μ L of product solution 05,1,2,3,4, inject liquid chromatograph, measure.Using concentration as abscissa, peak area is ordinate, is drawn bent
Line, obtain regression equation：Y=54695+66999 × 106X, r=09998, Isopsoralen is between 00342~02736 μ g
In good linear relationship, precision test, precision draws the μ L of reference substance solution 1, and sample introduction measure is repeated by above-mentioned chromatographic condition,
Isopsoralen peak area average product score value is 493247 (N=5）, RSD 107%.27 reappearance tests, with a collection of
Number sample, respectively determine 5 times, it is 0239%, RSD 205% to measure Isopsoralen content average value.Recovery test,
Oteoporosis treating medicinal capsule content 24mg is taken, it is accurately weighed, put in conical flask with cover, precision draws reference substance solution 1mL, by test sample
Method under solution preparation is prepared and determined, and sample measure, is determined according to method of drafting.
Goal of the invention：The compound preparation that oteoporosis treating medicinal capsule is made up of kinds of traditional Chinese medicines such as barrenwort, psoralea corylifolia, the fruit of glossy privets,
There is certain curative effect to climacteric women osteoporosis.Psoralea corylifolia is one of monarch drug in a prescription in side, its main component be psoralen with
Isopsoralen, both contents can be measured using high performance liquid chromatography, because of vacant psoralen reference substance, this reality
Test and only the Isopsoralen content in preparation is determined.
Technical scheme：The preparation of reference substance solution, precision weigh Isopsoralen reference substance 171mg, put in 25mL measuring bottles,
Add methanol to dissolve and be diluted to scale, shake up, produce and (contain Isopsoralen 00684mg per 1mL).The preparation of need testing solution,
Oteoporosis treating medicinal capsule content 50mg is taken, it is accurately weighed, put in conical flask with cover, precision adds methanol 25mL, weighed weight, ultrasound
20min is handled, is let cool, then weighed weight, less loss weight is supplied with methanol, is shaken up.Filtered with miillpore filter, take subsequent filtrate i.e.
.Chromatographic condition, methanol-water (V methanol: V water=48: 52)；Flow velocity 11mL/min；40 DEG C of column temperature；Wavelength 245nm.Measure side
Method, it is accurate respectively to draw μ L of reference substance solution 1, the μ L of need testing solution 15, liquid chromatograph is injected, measure, produces result.Different benefit
Bone fat element is good (r=0.9998) in 0.0342~0.2736 μ g linear relationships, average recovery rate be 92.11% (RSD=189%,
N=5), method favorable reproducibility (RSD=205%).
Invention beneficial effect：Isopsoralen content in oteoporosis treating medicinal capsule is detected with high performance liquid chromatography, can be avoided
The interference of other chemical compositions in preparation, specificity is good, and easy to operate.
Preferred forms：With detection and analysis.
Innovation：The new patent of invention of this item is related to a kind of assay side of Isopsoralen in oteoporosis treating medicinal capsule
Method, the compound preparation that oteoporosis treating medicinal capsule is made up of kinds of traditional Chinese medicines, Isopsoralen contained therein into belonging to Coumarins,
Due to containing benzo α pyranone parent nucleus in structure, UV absorption can be produced, therefore select high performance liquid chromatography to separate it
With detection.Experiment chromatogram shows that the component in negative control solution does not disturb the measure of Isopsoralen in preparation, the side of explanation
The specificity of method is good.
Claims (3)
1. the content assaying method of Isopsoralen in a kind of oteoporosis treating medicinal capsule, precision weigh Isopsoralen 171mg, put 25mL
In measuring bottle, add methanol to dissolve and be diluted to scale, shake up and produce and (contain Isopsoralen 0.0684mg per 1mL)；Bone is taken to dredge clever glue
Intracapsular tolerant 50mg, it is accurately weighed, addition methanol 25mL in conical flask with cover is put, weighed weight, 20min is ultrasonically treated, lets cool,
Weighed weight again, less loss weight is supplied with methanol, is shaken up；Filtered with miillpore filter, take subsequent filtrate to produce；Chromatographic condition, methanol
Water (V methanol: V water=48: 52)；Flow velocity 11mL/min；40 DEG C of column temperature；Wavelength 245nm；Assay method, respectively accurate absorption pair
According to μ L of product solution 1, the μ L of need testing solution 15, liquid chromatograph is injected, measure, produces result.
2. the method according to claim 11, it is characterized in that：Addition methanol 25mL in conical flask with cover is put, weighed weight, is surpassed
Sonication 20min, lets cool, then weighed weight, supplies less loss weight with methanol, shakes up；Filtered with miillpore filter, take subsequent filtrate i.e.
；Chromatographic condition, methanol-water (V methanol: V water=48: 52)；Flow velocity 11mL/min；40 DEG C of column temperature；Wavelength 245nm；Measure side
Method, it is accurate respectively to draw μ L of reference substance solution 1, the μ L of need testing solution 15, liquid chromatograph is injected, measure, produces result.
3. the method according to claim 11, it is characterized in that：Filtered with miillpore filter, take subsequent filtrate to produce；Chromatographic condition,
Methanol-water (V methanol: V water=48: 52)；Flow velocity 11mL/min；40 DEG C of column temperature；Wavelength 245nm；Assay method is accurate respectively to inhale
μ L of reference substance solution 1, the μ L of need testing solution 15 are taken, liquid chromatograph is injected, measure, produces result.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610721302.7A CN107782830A (en) | 2016-08-25 | 2016-08-25 | The content assaying method of Isopsoralen in a kind of oteoporosis treating medicinal capsule |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610721302.7A CN107782830A (en) | 2016-08-25 | 2016-08-25 | The content assaying method of Isopsoralen in a kind of oteoporosis treating medicinal capsule |
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| Publication Number | Publication Date |
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| CN107782830A true CN107782830A (en) | 2018-03-09 |
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| CN201610721302.7A Pending CN107782830A (en) | 2016-08-25 | 2016-08-25 | The content assaying method of Isopsoralen in a kind of oteoporosis treating medicinal capsule |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109085258A (en) * | 2018-07-10 | 2018-12-25 | 中山市中医院（广州中医药大学附属中山中医院） | A kind of quality determining method of Ficus lyrata |
| CN109342583A (en) * | 2018-09-29 | 2019-02-15 | 景宁畲族自治县食品药品检验检测中心 | It is a kind of it is small it is fragrant hook in psoralen and flavones content detection method |
-
2016
- 2016-08-25 CN CN201610721302.7A patent/CN107782830A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109085258A (en) * | 2018-07-10 | 2018-12-25 | 中山市中医院（广州中医药大学附属中山中医院） | A kind of quality determining method of Ficus lyrata |
| CN109342583A (en) * | 2018-09-29 | 2019-02-15 | 景宁畲族自治县食品药品检验检测中心 | It is a kind of it is small it is fragrant hook in psoralen and flavones content detection method |
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Application publication date: 20180309 |