CN101972323B - Quality analysis method for loins-strengthening and kidney-invigorating oral liquid - Google Patents
Quality analysis method for loins-strengthening and kidney-invigorating oral liquid Download PDFInfo
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- CN101972323B CN101972323B CN2010102819300A CN201010281930A CN101972323B CN 101972323 B CN101972323 B CN 101972323B CN 2010102819300 A CN2010102819300 A CN 2010102819300A CN 201010281930 A CN201010281930 A CN 201010281930A CN 101972323 B CN101972323 B CN 101972323B
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Abstract
The invention discloses a quality analysis method for loins-strengthening and kidney-invigorating oral liquid. The content of formononetin is measured by high performance liquid chromatography (HPLC), and the method comprises the steps of: preparing test solution, preparing reference solution and measuring. The method controls quality of the loins-strengthening and kidney-invigorating oral liquid by measuring the content of formononetin in the loins-strengthening and kidney-invigorating oral liquid through the HPLC, has high sensitivity, high specificity, no interference on negative control, has the accuracy, repeatability, linear relation and stability which can meet the requirements of scientific research and production, can more effectively control the product quality, and ensures the curative effect of medicaments.
Description
Technical field
The invention belongs to the field of quality control of Chinese medicine preparation, particularly a kind of mass analysis method of oral liquid for strengthening waist and kidney.
Background technology
Oral liquid for strengthening waist and kidney in the market generally by the oral liquid of flavour of a drug through being processed into such as reticulate millettia, rhizoma cibotii, parasitic loranthus, the fruit of Cherokee rose, the fruit of glossy privets, has loins-strengthening and kidney-invigorating, the effect of dispelling, collateral-activating; Be used for the deficiency of the kidney pain in the back; Treating rheumatic ostealgia, knee is soft unable, frequent urination.Clinical verification shows that this product is treated the efficient of Low Back Pain patient of suffering from a deficiency of the kidney and reached 95.0%, obvious effective rate 58.3%; The efficient of lumbar vertebrae hyperosteogeny patient reached 94.8%, the aching and limp clinical symptoms such as weak of soreness of waist distending pain, limbs pain, knee is all had significantly improvement effect.The reticulate millettia medicinal material has and enriches blood in the prescription, invigorate blood circulation, and the effect of vein relaxing, large usage quantity is a ministerial drug in the side.Yet pseudo-article are more on the reticulate millettia medicinal material market, and true and false difficulty is distinguished, therefore, need carry out quality control to the key component in the reticulate millettia, could guarantee quality, the guarantee curative effect of product.
Onocerin is one of principal ingredient in the reticulate millettia; At present few about the bibliographical information of the assay of onocerin; " content of onocerin in the high effective liquid chromatography for measuring Radix Astragali extract oral liquid " like people's report such as the 13rd volume the 1st phase Ji Gangfeng " traditional Chinese medicine Leader " in January, 2007; " Shenyang Pharmaceutical University's journal " " the RP-HPLC method is measured the content of onocerin in the reticulate millettia " that Dec in 2009, the 26th volume the 12nd phase Li Ying reported, the literary compositions such as " measuring the content of onocerin in the Spatholobi Paste with the HPLC method " that " number reason medical magazine " the 21st volume the 6th phase Xu Qing in 2008 etc. report.Adopt the method for distilling of bibliographical information that oral liquid for strengthening waist and kidney is extracted, the result shows: impurity is more in the sample, disturbs greatlyyer, can't detect onocerin, and chromatographic peak can't reach baseline separation.This is that contained medicinal material is different because product is different, and composition interferes with each other between the medicinal material, and the bibliographical information method prepares and measures, and can't obtain desirable separating effect.Therefore the assay that increases this composition can make this product quality more guaranteed, and curative effect is more definite.
Summary of the invention
The objective of the invention is to overcome the above-mentioned deficiency of prior art, providing a kind of can be the method that content carries out the composition measurement of index property to onocerin in the oral liquid for strengthening waist and kidney effectively, thereby more effectively controls the quality of this product.
For realizing above-mentioned purpose, the present invention has taked following technical scheme:
A kind of mass analysis method of oral liquid for strengthening waist and kidney adopts HPLC to measure the content of onocerin, may further comprise the steps:
A. prepare need testing solution
Get oral liquid for strengthening waist and kidney 40ml, add Petroleum ether extraction 2～3 times, each 40～80ml discards sherwood oil; Add methenyl choloride again and extract 2～3 times, each 40～80ml merges extract, volatilizes, and residue adds methanol constant volume to 10ml, shakes up, and filters, and promptly gets;
B. prepare reference substance solution
Get the onocerin reference substance, add methyl alcohol and process the solution that 1ml contains onocerin 20 μ g, promptly get;
C. measure
Chromatographic condition: with the octadecylsilane chemically bonded silica is filling agent, is that 38～42: 58～62 acetonitrile-1% formic acid solution is a moving phase with volume ratio; The detection wavelength is 290nm; Number of theoretical plate calculates by the onocerin peak should be not less than 4000;
Accurate respectively reference substance solution and the need testing solution 20 μ l of drawing inject liquid chromatograph, measure, and promptly get; Calculate according to the oral liquid for strengthening waist and kidney finished product, every milliliter of finished product contains onocerin, and to be no less than setting value be qualified.
Preferably, said step a is: get oral liquid for strengthening waist and kidney 40ml, add Petroleum ether extraction 2～3 times, each 60ml discards sherwood oil; Add methenyl choloride again and extract 2～3 times, each 60ml merges extract, volatilizes, and residue adds methanol constant volume to 10ml, shakes up, and filters, and is need testing solution.Moving phase described in the step c is that volume ratio is 40: 60 acetonitrile-1% formic acid solution.
Preferably, calculate according to the oral liquid for strengthening waist and kidney finished product, every milliliter of setting value that contains onocerin is 2 μ g.
Compared with prior art, the present invention has following beneficial effect:
The present invention adopts HPLC to measure the quality of the content of onocerin in the oral liquid for strengthening waist and kidney with the control oral liquid for strengthening waist and kidney; Highly sensitive; Specificity is strong, and negative control is noiseless, and its accuracy, reappearance, linear relationship, stability all can reach the requirement of research and production; Can more effectively control the quality of product, guarantee the curative effect of medicine.
Embodiment
Below specify the present invention through specific embodiment.
The mass analysis method of 1 one kinds of oral liquid for strengthening waist and kidney of embodiment
Adopt HPLC to measure the content of onocerin, may further comprise the steps:
A. prepare need testing solution
Get oral liquid for strengthening waist and kidney 40ml, add Petroleum ether extraction 2～3 times, each 60ml discards sherwood oil; Add methenyl choloride again and extract 2～3 times, each 60ml merges extract, volatilizes, and residue adds methanol constant volume to 10ml, shakes up, and filters, as need testing solution;
B. prepare reference substance solution
Get the onocerin reference substance, add methyl alcohol and process the solution that 1ml contains onocerin 20 μ g, promptly get reference substance solution;
C. measure
Chromatographic condition: with the octadecylsilane chemically bonded silica is filling agent, is that 38～42: 58～62 acetonitrile-1% formic acid solution is a moving phase with volume ratio; The detection wavelength is 290nm; Number of theoretical plate calculates by the onocerin peak should be not less than 4000;
Accurate respectively reference substance solution and the need testing solution 20 μ l of drawing inject liquid chromatograph, measure, and promptly get; Calculate according to the oral liquid for strengthening waist and kidney finished product, every milliliter contains onocerin and is no less than 2 μ g.
Get 8 lot sample article, carry out the onocerin assay, measure result such as table 1 according to the method for this embodiment.
Table 1
The conditional filtering of the mass analysis method of 2 one kinds of oral liquid for strengthening waist and kidney of embodiment and methodology checking
1.HPLC chromatographic condition screening
Existing bibliographical information has absorption at 249nm, 254nm place, and the spectrogram of measuring through PDAD shows at 249nm, 254nm, 290nm, 327nm place absorption is arranged all; Absorption maximum is 290nm, and is highly sensitive under this wavelength, and the peak type is sharp-pointed, degree of separation is greater than 1.5; Appearance time is in 10 minutes; Practice thrift detection time, so confirm that chromatographic condition is following: with the octadecylsilane chemically bonded silica is filling agent, and with 38～42: 58～62 acetonitrile-1% formic acid solution is a moving phase; The detection wavelength is 290nm.Number of theoretical plate calculates by the onocerin peak should be not less than 4000.
2. the preparation of test sample
Report in the list of references 1 " content of onocerin in the high effective liquid chromatography for measuring Radix Astragali extract oral liquid ", with the macroporous adsorptive resins adsorption sample, water and ethanol elution discard eluent respectively, continue and use methanol-eluted fractions, collect eluent.Report in the list of references 2 " the RP-HPLC method is measured the content of onocerin in the reticulate millettia " is with the methanol eddy sample.Report in the list of references 3 " measuring the content of onocerin in the Spatholobi Paste with the HPLC method " directly extracts sample, methanol constant volume with ethyl acetate.But by the sample of above-mentioned several kinds of literature methods preparation, all impurity is too many, can't detect onocerin.
Through a large amount of experiments, the final method of confirming to extract sample: Petroleum ether extraction 2～3 times, each 60ml discards sherwood oil; Add methenyl choloride again and extract 2～3 times, each 60ml merges extract, volatilizes, and residue adds methanol constant volume.The test liquid that according to said method prepares, impurity peaks is less in the chromatogram, and onocerin peak shape symmetry is good, noiseless.
3. methodology checking:
(1) linear relationship
It is an amount of to get the onocerin reference substance; The accurate title, decide; Processing the solution that contains onocerin 3.9 μ g/ml, 19.6 μ g/ml, 39.3 μ g/ml, 78.6 μ g/ml, 157.2 μ g/ml, 196.5 μ g/ml respectively with methyl alcohol, respectively get 20 μ l and inject liquid chromatograph, is ordinate with peak area (Y); The concentration of onocerin reference substance (X) is horizontal ordinate; The drawing standard curve, its regression equation is: Y=21143X-8.9284 (r=1), test shows that the onocerin reference substance is the good linear relation in 3.9～196.5 μ g/ml scopes.Regression equation is seen table 2:
Table 2
| The material title | Regression equation | R | The range of linearity |
| Onocerin | Y＝21143X-8.9284 | 1 | 3.9～196.5μg/ml |
(2) specificity test
Form and ratio in prescription; Take by weighing and remove the reticulate millettia medicinal material, the oral liquid for strengthening waist and kidney negative sample of processing according to the preparation method, and process negative controls by the need testing solution preparation method; Sample introduction in accordance with the law; The negative control chromatogram is illustrated under the experiment condition not having absorption peak with contrast onocerin place, in the prescription in other medicinal material composition noiseless to measuring the result.
(3) precision test
Accurate same sample solution 10 μ l, continuous sample introduction 6 times, the record chromatogram peak area, and the mean value and the RSD% of calculating onocerin peak area drawn.The result sees table 3, and onocerin peak area RSD% is 0.46, and the result shows that precision is good.
Table 3
| Measure number of times | 1 | 2 | 3 | 4 | 5 | 6 | Mean value | RSD(％) |
| The onocerin peak area | 334.63 | 335.61 | 336.43 | 335.12 | 337.84 | 338.52 | 336.36 | 0.46 |
(4) stability test
The same sample solution 10 μ l of accurate absorption, respectively at 0,2,4,6,8,12 hour sample introduction, record chromatogram peak area, and the mean value and the RSD% of calculating onocerin peak area.The result sees table 4, and onocerin peak area RSD% is 0.80, and the result shows that sample solution is stable in 12 hours.
Table 4
| Minute (h) | 0 | 2 | 4 | 6 | 8 | Mean value | RSD(％) |
| The onocerin peak area | 334.63 | 335.12 | 336.24 | 339.66 | 340.59 | 337.25 | 0.80 |
(5) replica test
Get the sample of same lot number, press the operation of sample determination method, measure content, the result sees table 5, and onocerin peak area RSD% is 2.53, and the result shows: this method reappearance is good.
Table 5
(6) recovery test
Adopt the application of sample absorption method, precision takes by weighing 6 parts in same sample, in every part, adds the onocerin contrast in right amount respectively, presses method operation under the assay item, measures, and calculates average recovery rate and RSD% value.The result sees table 6, and the onocerin average yield is 97.47%, and RSD is 0.75%.
Table 6
More than be to the specifying of possible embodiments of the present invention, but this embodiment is not in order to limiting claim of the present invention, does not allly break away from equivalence of the present invention and implement or change, all should be contained in the claim of the present invention.
Claims (4)
1. the mass analysis method of an oral liquid for strengthening waist and kidney is characterized in that, adopts HPLC to measure the content of onocerin, may further comprise the steps:
A. prepare need testing solution
Get oral liquid for strengthening waist and kidney 40ml, add Petroleum ether extraction 2～3 times, each 40～80ml discards sherwood oil; Add methenyl choloride again and extract 2～3 times, each 40～80ml merges extract, volatilizes, and residue adds methanol constant volume to 10ml, shakes up, and filters, and promptly gets;
B. prepare reference substance solution
Get the onocerin reference substance, add methyl alcohol and process the solution that 1ml contains onocerin 20 μ g, promptly get;
C. measure
Chromatographic condition: with the octadecylsilane chemically bonded silica is filling agent, is that 38～42: 58～62 acetonitrile-1% formic acid solution is a moving phase with volume ratio; The detection wavelength is 290nm; Number of theoretical plate calculates by the onocerin peak should be not less than 4000;
Accurate respectively reference substance solution and the need testing solution 20 μ l of drawing inject liquid chromatograph, measure, and promptly get; Calculate according to the oral liquid for strengthening waist and kidney finished product, every milliliter of finished product contains onocerin, and to be no less than setting value be qualified.
2. the mass analysis method of oral liquid for strengthening waist and kidney according to claim 1 is characterized in that, said step a is: get oral liquid for strengthening waist and kidney 40ml, add Petroleum ether extraction 2～3 times, each 60ml discards sherwood oil; Add methenyl choloride again and extract 2～3 times, each 60ml merges extract, volatilizes, and residue adds methanol constant volume to 10ml, shakes up, and filters, and is need testing solution.
3. the mass analysis method of oral liquid for strengthening waist and kidney according to claim 1 is characterized in that, moving phase described in the step c is that volume ratio is 40: 60 acetonitrile-1% formic acid solution.
4. according to the mass analysis method of each described oral liquid for strengthening waist and kidney of claim 1-3, it is characterized in that calculate according to the oral liquid for strengthening waist and kidney finished product, every milliliter of setting value that contains onocerin is 2 μ g.
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| CN115105552B (en) * | 2021-03-18 | 2024-01-12 | 河北百善药业有限公司 | Preparation method of large-sized waist-strengthening kidney-strengthening tablet |
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