CN106770708B - Determine whether psoralea corylifolia passes through the method for frying - Google Patents
Determine whether psoralea corylifolia passes through the method for frying Download PDFInfo
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Abstract
The embodiment of the invention provides a kind of methods whether determining psoralea corylifolia passes through frying, it include: that (1) weighs Malaytea Scurfpea Fruit, it is extracted with low concentration alcohol, obtains the first test solution, the concentration of measurement Psoralenoside, psoralen or Isopsoralenoside, Isopsoralen；Malaytea Scurfpea Fruit is weighed, is extracted with high concentration alcohol, the second test solution, the concentration of measurement Psoralenoside, psoralen or Isopsoralenoside, Isopsoralen are obtained；(2) calculate separately Psoralenoside, psoralen, Isopsoralenoside, Isopsoralen concentration and concentration in the second test solution in the first test solution ratio S1, S2, T1, T2, in the case where 0.9≤S1≤1.1 and S2≤1.1, or in the case where 0.9≤T1≤1.1 and T2≤1.1, determine the psoralea corylifolia by frying.Method provided in an embodiment of the present invention can effectively identify whether psoralea corylifolia passes through frying.
Description
Technical field
The present invention relates to technical field of traditional Chinese medicine preparation, and the side of frying whether is passed through more particularly to a kind of determining psoralea corylifolia
Method.
Background technique
Psoralea corylifolia is the fruit of legumes psoraleae, is China's traditional Chinese medicine, clinical application is extensive.Psoralea corylifolia has temperature
Effect that kidney is supporing yang, gas of receiving is relievingd asthma, warming spleen and stopping diarrha, interior treatment waist and knee crymodynia, spermatorrhoea, the enuresis, cold of insufficiency type cough, external curing are white
Purplish or white patches on the skin wind.Modern pharmacological studies have shown that psoralea corylifolia have increase myocardial contractive power, enhancing immune, expansion blood vessel, antibacterial, it is antitumor,
Estrogen-like action.Contain 100 multiple compounds in document report psoralea corylifolia, mainly includes coumarin kind compound, flavonoids
Compound, monoterpene phenolic compound.
The processing procedure of psoralea corylifolia is recorded in Lei Gong's Treatise on Preparation and Broiling of Materia Medica earliest, and the concocted method being described is referred to as Thunder God
Method.On this basis, medical scholar inherits in practice and has developed the preparation methods such as the system of frying and salt, wherein the system of frying refer to by
Raw psoralea corylifolia is placed in frying container, be fried with slow fire it is micro- heave, have crack；Salt system refers to raw psoralea corylifolia is first at room temperature
It is placed in salt water and mixes thoroughly, it is bored, it is subsequently placed in frying container, mild fire heating, stir-fry is heaved to micro-, split and aromatic ease
Out.The system of either frying or salt system, psoralea corylifolia are required by this road technique of frying.It therefrom medically says, raw psoralea corylifolia temperature
Kidney effect is strong, uses impairment of yin for a long time；And the effect of warm positive antidiarrheal can be enhanced after psoralea corylifolia frying.
Currently, the life psoralea corylifolia of each medicinal material market, frying psoralea corylifolia and salt psoralea corylifolia processed and obscuring seriously；Part medicine materical crude slice factory
For save the cost, sold using raw psoralea corylifolia as psoralea corylifolia or salt psoralea corylifolia processed is fried, this way does not meet Chinese medicine
Concocted specification, and reduction the effect of may result in psoralea corylifolia.And do not report effectively whether identify psoralea corylifolia in document
By the method for frying.
Summary of the invention
Inventor has now surprisingly been found that by extensive research, without the psoralea corylifolia of frying, uses alcohol molten as extracting
Agent extracts, and in the solution obtained after extraction, the concentration of Psoralenoside and Isopsoralenoside is with the alcohol in Extraction solvent
Concentration is reduced and is reduced, and the concentration of psoralen and isopsorapen is increased as the concentration of the alcohol in Extraction solvent reduces；
And the psoralea corylifolia Jing Guo frying, use alcohol to extract as Extraction solvent, in the solution obtained after extraction, psoralen and different benefit
The concentration of bone fat element is reduced as the concentration of the alcohol in Extraction solvent reduces, and the concentration of Psoralenoside and Isopsoralenoside is basic
It is constant.Based on this, the embodiment of the invention discloses a kind of methods whether determining psoralea corylifolia passes through frying, mend for effectively identifying
Whether bone fat passes through frying.Specific technical solution is as follows:
Whether a kind of determining psoralea corylifolia passes through the method for frying, which comprises
(1) Malaytea Scurfpea Fruit that quality is M1 is weighed, is extracted with the low concentration alcohol that volume is V1, obtains first for examination
Product solution measures Psoralenoside, the concentration of psoralen or Isopsoralenoside, Isopsoralen in first test solution
Concentration；
The Malaytea Scurfpea Fruit that quality is M2 is weighed, the high concentration alcohol for being V2 with volume extracts, and obtains the second test sample
Solution measures Psoralenoside, the concentration of psoralen or Isopsoralenoside in second test solution, Isopsoralen
Concentration；
Wherein, M2:V2=M1:V1, the high concentration alcohol are the alcohol of concentration of volume percent >=75%, the high concentration alcohol
With difference >=25% of the percent concentration of the low concentration alcohol；
(2) Psoralenoside is calculated in the ratio of concentration and the concentration in the second test solution in the first test solution
Value S1, and psoralen is calculated in the ratio of concentration and the concentration in the second test solution in the first test solution
S2；
In the case where 0.9≤S1≤1.1 and S2≤1.1, determine the psoralea corylifolia by frying；
Or
Isopsoralenoside is calculated in the ratio of concentration and the concentration in the second test solution in the first test solution
Value T1, and Isopsoralen is calculated in the ratio of concentration and the concentration in the second test solution in the first test solution
T2；
In the case where 0.9≤T1≤1.1 and T2≤1.1, determine the psoralea corylifolia by frying.
In the preferred embodiment of the present invention, the alcohol is at least one of methanol, ethyl alcohol.
It is more highly preferred in embodiment in one kind of the invention, the low concentration alcohol is concentration of volume percent≤60%
Alcohol, the alcohol that preferred volume percent concentration is 50%.
It is more highly preferred in embodiment in one kind of the invention, it is 100% that the high concentration alcohol, which is concentration of volume percent,
Alcohol.
It is more highly preferred in embodiment in one kind of the invention, M1:V1 is 1mg/mL~20mg/mL.
It is more highly preferred in embodiment in one kind of the invention, in step (1), institute is measured using ultra performance liquid chromatography
State Psoralenoside, the concentration of psoralen or Isopsoralenoside in the first test solution and second test solution, different
The concentration of psoralen.
It is more highly preferred in embodiment in one kind of the invention, the default chromatographic condition of ultra performance liquid chromatography includes:
Chromatographic column: using the stationary phase of octadecylsilane chemically bonded silica；Mobile phase: A phase is 0.01%~1% formic acid water
Solution, B phase are methanol；Gradient elution, the gradient elution specifically: methanol accounts for the percent by volume of mobile phase in following ranges
Inside increase as time increases, 0 minute~6 minutes, 10%~60%.
It is more highly preferred in embodiment in one kind of the invention, the default chromatographic condition of ultra performance liquid chromatography further include:
Column temperature: 50 DEG C~70 DEG C；Flow velocity: 0.1mL/ minutes~0.5mL/ minutes；Detection wavelength: 246nm~254nm；Into
Sample amount: 1 μ of μ L~5 L.
Be more highly preferred in embodiment in one kind of the invention, it is described be extracted as ultrasonic extraction, in refluxing extraction at least
It is a kind of.
The present invention provides a kind of methods whether determining psoralea corylifolia passes through frying, respectively with the alcohol pair of two kinds of various concentrations
Psoralea corylifolia extracts, and obtains two kinds of test solutions, then measures Psoralenoside, psoralen in two kinds of test solutions
Concentration or Isopsoralenoside, Isopsoralen concentration, according to concentration of the Psoralenoside in the first test solution with
The ratio S1 of concentration in second test solution, concentration of the psoralen in the first test solution in the second test sample
The ratio S2 or Isopsoralenoside of concentration in solution are in the concentration in the first test solution and in the second test solution
The ratio T1 of concentration, Isopsoralen is in the concentration in the first test solution and the concentration in the second test solution
Ratio T2, identifies whether psoralea corylifolia passes through frying.Because without the value of S1, S2 of the psoralea corylifolia of frying and the benefit Jing Guo frying
The value of S1, S2 of bone fat be it is different, without the value of T1, T2 of the psoralea corylifolia of frying and the psoralea corylifolia Jing Guo frying
The value of T1, T2 are also different, so can effectively identify whether psoralea corylifolia passes through frying by the above method.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
It obtains other drawings based on these drawings.
Fig. 1 is when extracting raw psoralea corylifolia using the methanol of various concentration in the embodiment of the present invention 1, four kinds in test solution
The concentration map of index components Psoralenoside, psoralen, Isopsoralenoside, Isopsoralen；
Fig. 2 is when frying psoralea corylifolia processed using the methanol extraction of various concentration in the embodiment of the present invention 2, in test solution
The concentration map of four kinds of index components；
Fig. 3 is the ultra performance liquid chromatography figure of the first test solution of sample 1 in the embodiment of the present invention 3；
Fig. 4 is the ultra performance liquid chromatography figure of the second test solution of sample 1 in the embodiment of the present invention 3.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
The embodiment of the invention discloses a kind of methods whether determining psoralea corylifolia passes through frying, comprising:
(1) Malaytea Scurfpea Fruit that quality is M1 is weighed, is extracted with the low concentration alcohol that volume is V1, obtains first for examination
Product solution measures Psoralenoside, the concentration of psoralen or Isopsoralenoside, Isopsoralen in first test solution
Concentration；
The Malaytea Scurfpea Fruit that quality is M2 is weighed, the high concentration alcohol for being V2 with volume extracts, and obtains the second test sample
Solution measures Psoralenoside, the concentration of psoralen or Isopsoralenoside in second test solution, Isopsoralen
Concentration；
Wherein, M2:V2=M1:V1, the high concentration alcohol are the alcohol of concentration of volume percent >=75%, the high concentration alcohol
With difference >=25% of the percent concentration of the low concentration alcohol；
(2) Psoralenoside is calculated in the ratio of concentration and the concentration in the second test solution in the first test solution
Value S1, and psoralen is calculated in the ratio of concentration and the concentration in the second test solution in the first test solution
S2；
In the case where 0.9≤S1≤1.1 and S2≤1.1, determine the psoralea corylifolia by frying；
Or
Isopsoralenoside is calculated in the ratio of concentration and the concentration in the second test solution in the first test solution
Value T1, and Isopsoralen is calculated in the ratio of concentration and the concentration in the second test solution in the first test solution
T2；
In the case where 0.9≤T1≤1.1 and T2≤1.1, determine the psoralea corylifolia by frying.
By the psoralea corylifolia of frying, alcohol is used to extract as Extraction solvent, in the solution obtained after extraction, psoralen
It is reduced with the concentration of Isopsoralen as the concentration of the alcohol in Extraction solvent reduces, the concentration difference of alcohol is bigger, psoralea corylifolia
The concentration difference of element and Isopsoralen is also bigger；The concentration of Psoralenoside and Isopsoralenoside is basically unchanged.
And without the psoralea corylifolia of frying, use alcohol to extract as Extraction solvent, in the solution obtained after extraction, four kinds
The concentration variation tendency of index components is then different, specifically, the concentration of Psoralenoside and Isopsoralenoside is in Extraction solvent
The concentration of alcohol reduce and reduce, the concentration of psoralen and isopsorapen with the concentration reduction of the alcohol in Extraction solvent and
It increases；The concentration difference of alcohol is bigger, and the concentration difference of four kinds of index components is also bigger；But this variation tendency is in the volume of alcohol
It is more obvious when percent concentration >=50%, when the concentration of volume percent of alcohol is less than 50%, the concentration of four kinds of index components
It is basically unchanged.
For above-mentioned two classes psoralea corylifolia, although in the solution obtained after extracting, the concentration variation tendency of four kinds of index components
Difference, but if the concentration difference of alcohol is too small in Extraction solvent, two kinds of variation tendencies also cannot be distinguished, i.e., can not determine Psoralen
Whether rouge passes through frying；And it if the concentration of volume percent of the pure and mild low concentration alcohol of high concentration is smaller, such as is respectively less than
50%, then also it is difficult to distinguish two kinds of variation tendencies, that is, is difficult to determine whether psoralea corylifolia passes through frying.Therefore, the embodiment of the present invention
Concentration of volume percent >=75% of middle and high concentration alcohol, difference >=25% of the percent concentration of the pure and mild low concentration alcohol of high concentration.
In conjunction with above-mentioned rule, and in view of error existing for each link of discrimination process, the value range of S1, T1 are determined as by inventor
0.9~1.1, the value range of S2, T2 are determined as≤1.1.
Wherein, above-mentioned alcohol is preferably at least one of methanol, ethyl alcohol, it is furthermore preferred that above-mentioned alcohol is methanol.It is above-mentioned low dense
Degree alcohol be preferably concentration of volume percent≤60% alcohol, more preferably concentration of volume percent be 50% alcohol.Above-mentioned height
Concentration alcohol is preferably the alcohol that concentration of volume percent is 100%.M1:V1 is preferably 1mg/mL~20mg/mL.It extracts preferably super
At least one of sound extraction, refluxing extraction, in order to easy to operate, extraction is more preferably ultrasonic extraction.
In step (1), it is preferred to use ultra performance liquid chromatography measures the first test solution and the second test solution
The concentration of middle Psoralenoside, the concentration of psoralen or Isopsoralenoside, Isopsoralen.Wherein, ultra performance liquid chromatography
The preferably following condition of default chromatographic condition:
Chromatographic column: using the stationary phase of octadecylsilane chemically bonded silica；Mobile phase: A phase is 0.01%~1% formic acid water
Solution, B phase are methanol；Gradient elution, the gradient elution specifically: methanol accounts for the percent by volume of mobile phase in following ranges
Inside increase as time increases, 0 minute~6 minutes, 10%~60%.
It is furthermore preferred that the column temperature of the chromatographic column of ultra performance liquid chromatography is 50 DEG C~70 DEG C；Flow velocity be 0.1mL/ minutes~
0.5mL/ minutes；Detection wavelength is 246nm~254nm；Sample volume is 1 μ of μ L~5 L.
As seen from the above, it the embodiment of the invention provides a kind of method whether determining psoralea corylifolia passes through frying, uses respectively
The alcohol of two kinds of various concentrations extracts psoralea corylifolia, obtains two kinds of test solutions, then measures in two kinds of test solutions
Psoralenoside, the concentration of psoralen or the concentration of Isopsoralenoside, Isopsoralen, according to Psoralenoside first for examination
Concentration in product solution in the ratio S1 of the concentration in the second test solution, psoralen in the first test solution
Concentration in the concentration in the second test solution concentration in the first test solution of ratio S2 or Isopsoralenoside with
It is supplied in the ratio T1 of the concentration in the second test solution, concentration of the Isopsoralen in the first test solution and second
The ratio T2 of concentration in test sample solution, identifies whether psoralea corylifolia passes through frying.Because of S1, S2 of the psoralea corylifolia without frying
Value and the psoralea corylifolia Jing Guo frying S1, S2 value be it is different, without the value and warp of T1, T2 of the psoralea corylifolia of frying
It is also different for crossing the value of T1, T2 of the psoralea corylifolia of frying, so effectively whether can identify psoralea corylifolia by the above method
By frying.
Whether pass through the side of frying to a kind of determining psoralea corylifolia provided in an embodiment of the present invention below by specific embodiment
Method is described in detail.
During Examples 1 to 3 and following drafting standard curves, it is all made of ultra performance liquid chromatography and measures four kinds of fingers
The concentration of ingredient Psoralenoside, Isopsoralenoside, psoralen, Isopsoralen is marked, and used chromatographic condition is all the same,
Chromatographic condition is specific as follows:
Instrument: Waters ACQUITY UPLCTMSystem Ultra Performance Liquid Chromatography instrument；
Chromatographic column: (wherein the packing material size in chromatographic column is 1.7 μm to ACQUITY UPLC BEH C18, chromatography column internal diameter
For 2.1mm, column length 50mm)；
Column temperature: 60 DEG C, flow velocity: 0.3mL/ minutes, Detection wavelength: 246nm, sample volume: 2 μ L
Mobile phase: 0.1% aqueous formic acid-methanol, gradient elution, elution program are shown in Table 1.
The gradient elution program of 1 ultra performance liquid chromatography of table
The standard curve of the concentration of four kinds of index components Psoralenosides, Isopsoralenoside, psoralen, Isopsoralen
Drawing process, specific as follows:
Psoralenoside 5.21mg, Isopsoralenoside 5.15mg, psoralen 5.11mg, Isopsoralen 4.98mg are taken, essence
It is close weighed, it is respectively placed in 5mL volumetric flask, is dissolved with methanol (methanol that concentration of volume percent is 100%) and be settled to quarter
Degree, respectively obtain concentration be 1.04mg/mL Psoralenoside stock solution, concentration be 1.03mg/mL Isopsoralenoside stock solution,
The Isopsoralen stock solution that the psoralen stock solution and concentration that concentration is 1.02mg/mL are 1.00mg/mL, it is spare.Respectively
Each 400 μ L of Psoralenoside stock solution, Isopsoralenoside stock solution is taken, psoralen stock solution, Isopsoralen stock solution are each
1mL is placed in same 5mL volumetric flask, with methanol constant volume to scale, shakes up, and obtains hybrid standard product solution.Hybrid standard product are molten
In liquid, Psoralenoside concentration is 83.36 μ g/mL, Isopsoralenoside concentration is 82.40 μ g/mL, psoralen concentration is 204.4 μ
G/mL, Isopsoralen concentration are 199.2 μ g/mL.The methanol for being 30% with concentration of volume percent is by above-mentioned hybrid standard product
Solution dilutes 2,4,8,16,32,64 times step by step, obtains a series of hybrid standard product solution of various concentrations.Then superelevation is used
Effect liquid phase chromatogram is measured a series of hybrid standard product solution of above-mentioned various concentrations, obtains corresponding ultra high efficiency liquid phase color
Spectrogram.Respectively using Psoralenoside, Isopsoralenoside, psoralen, Isopsoralen concentration as abscissa, corresponding ultra high efficiency
The peak area of chromatographic peak is ordinate in liquid chromatogram, and drafting obtains four standard curves, the linear regression of each standard curve
Equation, the range of linearity, r2Value is shown in Table 2.
2 Psoralenoside of table, Isopsoralenoside, psoralen, the equation of linear regression of Isopsoralen, the range of linearity and r2
Value
Methanol concentration in 1 Test extraction solvent of embodiment is dense to four kinds of index components in raw psoralea corylifolia test solution
The influence of degree
(a) prepared by powder sample
Raw psoralea corylifolia (being purchased from Hebei Anguo medicinal material market) is crushed, raw Malaytea Scurfpea Fruit is obtained.
(b) test solution 1 of raw psoralea corylifolia is prepared:
Above-mentioned raw Psoralen is prepared using the extracting method of the psoralea corylifolia recorded in 2015 editions Pharmacopoeias of the People's Republic of China
The test solution 1 of rouge.Preparation process is specific as follows:
Above-mentioned raw Malaytea Scurfpea Fruit 0.5g is taken, it is accurately weighed, it is placed in Soxhlet extractor, adds methanol appropriate, be heated to reflux
It extracts 2 hours, is transferred in the volumetric flask of 100mL after being cooled to room temperature, adds methanol to scale, shake up, 14000rpm (revolutions per minute
Clock) centrifugation 10 minutes, supernatant 1mL is taken, the methanol aqueous solution that 1mL concentration of volume percent is 30% is then added, mixes, i.e.,
The test solution 1 of psoralea corylifolia must be given birth to.
(c) the test solution 2-6 of raw psoralea corylifolia is prepared:
Above-mentioned raw Malaytea Scurfpea Fruit 0.5g is taken, it is accurately weighed, it is placed in the volumetric flask of 100mL, adds proper amount of methanol, at 60 DEG C
Lower ultrasonic extraction 0.5 hour places to room temperature, is settled to scale, shakes up, and 14000rpm is centrifuged 10 minutes, takes supernatant 1mL,
Then the methanol aqueous solution that 1mL concentration of volume percent is 30% is added, mixes to get the test solution 2 of raw psoralea corylifolia.
The methanol of extraction in above-mentioned steps is changed to the first that concentration of volume percent is 75%, 50%, 25% respectively
Alcohol solution and water, repeat said extracted operation, obtain the test solution 3-6 of raw psoralea corylifolia respectively.
(d) four kinds of index components Psoralenosides, Isopsoralenoside, psoralen, different Psoralen in each test solution are measured
The concentration of rouge element:
To the test solution of above-mentioned six raw psoralea corylifolias, it is respectively adopted in ultra performance liquid chromatography measurement test solution
Six ultra performance liquid chromatography figures are obtained in the concentration of four kinds of index components.It is read from every ultra performance liquid chromatography figure respectively
The peak area for taking four kinds of index components brings the peak area of every kind of index components in table 2 in corresponding regression equation into, obtains each
The concentration C 1 (μ g/mL) of each index components in test solution.It should be noted that accurately weighed refer to that weighing quality answers accurately
To the one thousandth of taken quality.In view of it is accurately weighed when each sample powder quality difference, in order to make concentrations versus more
Accurately, above-mentioned concentration C 1 is converted into concentration C 2 (mmol/g) according to the following formula:
C2=(C1*2*100*10-3)/(M*m)
Wherein, M is the molecular weight of index components corresponding to C1, and m is that test solution corresponding to C1 is smart in the preparation
The quality of close weighed life psoralea corylifolia.
Then using the number of test solution as ordinate, the concentration C 2 of each index components is abscissa, and mapping obtains figure
1.From Fig. 1 it can be found that the test sample of the concentration of four kinds of index components and raw psoralea corylifolia is molten in the test solution 1 of raw psoralea corylifolia
The concentration of four kinds of index components is essentially identical in liquid 2, i.e., using ultrasonic extraction and using 2015 editions " People's Republic of China's medicines
Allusion quotation " in the extracting method of psoralea corylifolia that records raw psoralea corylifolia is extracted, obtained extraction result is consistent.In addition, from
Fig. 1 is it can be found that in the test solution of raw psoralea corylifolia, and the concentration of Psoralenoside and Isopsoralenoside is in Extraction solvent
The concentration of methanol is reduced and is reduced, the concentration of psoralen and isopsorapen with the methanol in Extraction solvent concentration reduction
And it increases；But the concentration of four kinds of index components and the test solution 6 for giving birth to psoralea corylifolia from the test solution 5 for giving birth to psoralea corylifolia
In the concentration of four kinds of index components be not much different, it can be found that the volume of above-mentioned concentration variation tendency methanol in Extraction solvent
It is more obvious when percent concentration >=50%.
Methanol concentration in 2 Test extraction solvent of embodiment to the four kinds of indexs fried in psoralea corylifolia test solution processed at
Divide the influence of concentration
(a) prepared by powder sample
Will raw psoralea corylifolia (being purchased from Hebei Anguo medicinal material market) be placed in frying container be fried with slow fire it is micro- heave, have crack
Sound then takes out crushing, obtains frying Malaytea Scurfpea Fruit processed.
(b) test solution 1 of psoralea corylifolia processed is fried in preparation:
The above-mentioned system of frying is prepared using the extracting method of the psoralea corylifolia recorded in 2015 editions Pharmacopoeias of the People's Republic of China
The test solution 1 of psoralea corylifolia.Preparation process is specific as follows:
Take it is above-mentioned fry Malaytea Scurfpea Fruit 0.5g processed, it is accurately weighed, be placed in Soxhlet extractor, add methanol appropriate, heat
It refluxing extraction 2 hours, is transferred in the volumetric flask of 100mL after being cooled to room temperature, adds methanol to scale, shake up, 14000rpm (turns
It is centrifuged 10 minutes per minute), takes supernatant 1mL, the methanol aqueous solution that 1mL concentration of volume percent is 30% is then added, mixes
It is even to get the test solution 1 for frying psoralea corylifolia processed.
(c) the test solution 2-6 of psoralea corylifolia processed is fried in preparation:
Take it is above-mentioned fry Malaytea Scurfpea Fruit 0.5g processed, it is accurately weighed, be placed in the volumetric flask of 100mL, add proper amount of methanol,
Ultrasonic extraction 0.5 hour at 60 DEG C places to room temperature, is settled to scale, shakes up, and 14000rpm is centrifuged 10 minutes, takes supernatant
Then 1mL is added the methanol aqueous solution that 1mL concentration of volume percent is 30%, mixes to get the test sample for frying psoralea corylifolia processed
Solution 2.
The methanol of extraction in above-mentioned steps is changed to the first that concentration of volume percent is 75%, 50%, 25% respectively
Alcohol solution and water repeat said extracted operation, obtain the test solution 3-6 for frying psoralea corylifolia processed respectively.
(d) four kinds of index components Psoralenosides, Isopsoralenoside, psoralen, different Psoralen in each test solution are measured
The concentration of rouge element:
It is molten that ultra performance liquid chromatography measurement test sample is respectively adopted in the test solution that above-mentioned six are fried with psoralea corylifolia processed
Six ultra performance liquid chromatography figures are obtained in the concentration of four kinds of index components in liquid.Respectively from every ultra performance liquid chromatography figure
The middle peak area for reading four kinds of index components, the peak area of every kind of index components is brought into table 2 in corresponding regression equation, is obtained
The concentration C 1 of each index components into each test solution.In view of it is accurately weighed when each sample powder quality difference, in order to
Keep concentrations versus more accurate, according to the reduction formula of concentration C 1 and concentration C 2 above-mentioned, concentration C 1 is converted into concentration C 2.
Then using the number of test solution as ordinate, the concentration C 2 of each index components is abscissa, and mapping obtains figure
2.From Fig. 2 it can be found that frying the concentration of four kinds of index components in the test solution 1 of psoralea corylifolia processed and frying psoralea corylifolia processed
The concentration of four kinds of index components is essentially identical in test solution 2, i.e., using ultrasonic extraction and use 2015 editions, " the Chinese people are total
With state's pharmacopeia " in the extracting method of psoralea corylifolia that records extracted to psoralea corylifolia processed is fried, obtained extraction result is also one
It causes.In addition, from Fig. 2 it can be found that frying in the test solution of psoralea corylifolia processed, the concentration of psoralen and isopsorapen
It as the concentration of the methanol in Extraction solvent reduces and reduces, the concentration of Psoralenoside and Isopsoralenoside is basically unchanged.
From embodiment 1 and embodiment 2 as it can be seen that without frying psoralea corylifolia, use alcohol to extract as Extraction solvent, mention
In the solution obtained after taking, the concentration of Psoralenoside and Isopsoralenoside is dropped as the concentration of the alcohol in Extraction solvent reduces
Low, the concentration of psoralen and isopsorapen is increased as the concentration of the alcohol in Extraction solvent reduces；And pass through frying
Psoralea corylifolia uses alcohol to extract as Extraction solvent, in the solution obtained after extraction, the concentration of psoralen and isopsorapen
It as the concentration of the alcohol in Extraction solvent reduces and reduces, the concentration of Psoralenoside and Isopsoralenoside is basically unchanged.In addition, adopting
With ultrasonic extraction and using the psoralea corylifolia recorded in 2015 editions Pharmacopoeias of the People's Republic of China extracting method to psoralea corylifolia into
Row extracts, and obtained extraction result is consistent.Since ultrasonic extraction is easy to operate, in the actual operation process, extract
Method can preferred ultrasonic extraction.
Below by taking the methanol aqueous solution that methanol and concentration of volume percent are 50% as an example, to disclosed by the embodiments of the present invention
A kind of method whether determining psoralea corylifolia passes through frying is illustrated.
Embodiment 3 identifies whether nine kinds of samples pass through frying
The present embodiment specifically determines whether following nine kinds of psoralea corylifolia samples pass through frying.Shown in nine kinds of samples are specific as follows:
Sample 1: raw psoralea corylifolia (being purchased from Hebei Anguo medicinal material market)
Sample 2: sample 1 being placed in the salt water that concentration is 2%, and bored profit is dried after 12 hours at room temperature.
Sample 3: sample 1 being placed in the salt water that concentration is 2%, and bored profit is divided after 12 hours with mild fire frying 10 at room temperature
Clock.
Sample 4: raw psoralea corylifolia (being purchased from Hui nationality's medicinal material market)
Sample 5: sample 4 being placed in the salt water that concentration is 2%, and bored profit is dried after 12 hours at room temperature.
Sample 6: sample 4 being placed in the salt water that concentration is 2%, and bored profit is divided after 12 hours with mild fire frying 10 at room temperature
Clock.
Sample 7: raw psoralea corylifolia (being purchased from Guangxi medicinal material market)
Sample 8: sample 7 being placed in the salt water that concentration is 2%, and bored profit is dried after 12 hours at room temperature.
Sample 9: sample 7 being placed in the salt water that concentration is 2%, and bored profit is divided after 12 hours with mild fire frying 10 at room temperature
Clock.
Nine kinds of samples are divided into three groups and are detected, and are respectively as follows:
First group: sample 1-3, measure sample 1-3 the first test solution and the second test solution in Psoralenoside,
The concentration of psoralen；
Second group: sample 4-6, measure different psoralea corylifolia in the first test solution and the second test solution of sample 4-6
The concentration of glycosides, Isopsoralen；
Third group: sample 7-9, measure sample 7-9 the first test solution and the second test solution in Psoralenoside,
The concentration of psoralen, Isopsoralenoside, Isopsoralen；
Nine kinds of samples are smashed respectively, obtain the powder of sample 1-9.
Discrimination process is specific as follows by taking sample 1 as an example:
(1) 1 powder 0.5g of sample is taken, it is accurately weighed, it is placed in the volumetric flask of 100mL, adds appropriate volume percent concentration
For 50% methanol aqueous solution, ultrasonic extraction 0.5 hour at 60 DEG C places to room temperature, is settled to scale, shakes up,
14000rpm is centrifuged 10 minutes, takes supernatant 1mL, and the methanol aqueous solution that 1mL concentration of volume percent is 30% is then added, mixes
Even the first test solution to get sample 1.
1 powder 0.5g of sample is taken, it is accurately weighed, it is placed in the volumetric flask of 100mL, adds proper amount of methanol, it is ultrasonic at 60 DEG C
Extract 0.5 hour, place to room temperature, be settled to scale, shake up, 14000rpm is centrifuged 10 minutes, take supernatant 1mL, then plus
Enter the methanol aqueous solution that 1mL concentration of volume percent is 30%, mixes the second test solution to get sample 1.
It is measured using first test solution of the ultra performance liquid chromatography to sample 1, obtains the first of sample 1 for examination
The ultra performance liquid chromatography figure (Fig. 3) of product solution.By the comparison of the ultra performance liquid chromatography figure with standard solution, figure is learnt
It is the chromatographic peak of Psoralenoside that the chromatographic peak for being is marked in 3, and the chromatographic peak labeled as 2 is the chromatographic peak of Isopsoralenoside, label
Chromatographic peak for 3 is the chromatographic peak of psoralen, and the chromatographic peak labeled as 4 is the chromatographic peak of Isopsoralen.It obtains and is mended in Fig. 3
The chromatographic peak peak area of bone fat glycosides, psoralen brings in table 2 peak area of above two index components into accordingly recurrence side
Cheng Zhong obtains the concentration C 1 of Psoralenoside in the first test solution of sample 1, psoralen, is respectively labeled as C1- psoralea corylifolia
Glycosides, C1- psoralen.In view of it is accurately weighed when each sample powder quality difference, in order to keep the ratio of concentration more accurate,
According to the reduction formula of concentration C 1 and concentration C 2 above-mentioned, concentration C 1 is converted into concentration C 2, is respectively labeled as C2- psoralea corylifolia
Glycosides, C2- psoralen, C2- Psoralenoside=0.0139mmol/g, C2- psoralen=0.0524mmol/g.
Said determination step is repeated, the concentration of Psoralenoside, psoralen in the second test solution of sample 1 is obtained
C2 is respectively labeled as C2 '-Psoralenoside, C2 '-psoralen, C2 '-Psoralenoside=0.0326mmol/g, C2 '-psoralea corylifolia
Element=0.0352mmol/g.Wherein, the ultra performance liquid chromatography figure of the second test solution of sample 1 is as shown in Figure 4.
(2) basis
S1=C2- Psoralenoside/C2 '-Psoralenoside
S2=C2- psoralen/C2 '-psoralen
S1=0.426, S2=1.489 of sample 1 is calculated.
Because S1, S2 are unsatisfactory for the condition of 0.9≤S1≤1.1 and S2≤1.1, thus may determine that sample 1 is without stir-fry
System.This judging result is consistent with the actual conditions of sample 1.
Sample 2-9 is identified according to the method for above-mentioned identification sample 1, is respectively obtained
The C2- Psoralenoside of sample 2-3, C2- psoralen, C2 '-Psoralenoside, C2 '-psoralen value；
The C2- Isopsoralenoside of sample 4-6, C2- Isopsoralen, C2 '-Isopsoralenoside, C2 '-Isopsoralen value；
The C2- Psoralenoside of sample 7-9, C2- psoralen, C2 '-Psoralenoside, C2 '-psoralen, the different Psoralen of C2-
Rouge glycosides, C2- Isopsoralen, C2 '-Isopsoralenoside, C2 '-Isopsoralen value；
Specifically it is shown in Table 3-6.
The C2- Psoralenoside of 3 sample 2-3 of table, C2- psoralen, C2 '-Psoralenoside, C2 '-psoralen value
C2- Isopsoralenoside, C2- Isopsoralen, C2 '-Isopsoralenoside, the C2 '-Isopsoralen of 4 sample 4-6 of table
Value
The C2- Psoralenoside of 5 sample 7-9 of table, C2- psoralen, C2 '-Psoralenoside, C2 '-psoralen value
C2- Isopsoralenoside, C2- Isopsoralen, C2 '-Isopsoralenoside, the C2 '-Isopsoralen of 6 sample 7-9 of table
Value
According to
S1=C2- Psoralenoside/C2 '-Psoralenoside
S2=C2- psoralen/C2 '-psoralen
T1=C2- Isopsoralenoside/C2 '-Isopsoralenoside
T2=C2- Isopsoralen/C2 '-Isopsoralen
Respectively obtain S1, S2 value of sample 2-3, T1, T2 value of sample 4-6, S1, S2, T1, T2 value of sample 7-9, specifically
It is shown in Table 7.
S1, S2 or T1 of 7 sample 2-9 of table, T2 value
According to S1, S2 value of sample 2-3 in table 7, judgement sample 2 passes through frying without frying, sample 3.This judgement
As a result it is consistent with the actual conditions of sample 2-3.
According to T1, T2 value of sample 4-6 in table 7, judgement sample 4-5 passes through frying without frying, sample 6.This is sentenced
Disconnected result is consistent with the actual conditions of sample 4-6.
According to S1, S2 of sample 7-9 in table 7, judgement sample 7-8 passes through frying without frying, sample 9.According in table 7
T1, T2 value of sample 7-9 also can determine whether out sample 7-8 without frying, and sample 9 passes through frying.That is, either adopting
Judged with S1, S2 value, or is judged that judging result is consistent with the actual conditions of sample 7-9 using T1, T2 value
It closes.
It should be noted that in embodiment 3 by taking the methanol aqueous solution that methanol and concentration of volume percent are 50% as an example, really
Determine whether psoralea corylifolia passes through frying.However, it will be understood that dense in test solution according to aforementioned four kinds of index components
Changing rule is spent, using the alcohol of other two kinds of concentration, as long as meeting concentration of volume percent >=75% of high concentration alcohol, and highly concentrated
Difference >=25% of the percent concentration of pure and mild low concentration alcohol is spent, corresponding result can be obtained.
Therefore, as seen from the above, the side of frying whether is passed through using a kind of determining psoralea corylifolia provided in an embodiment of the present invention
Method can effectively identify whether psoralea corylifolia passes through frying.
It should be noted that, in this document, relational terms such as first and second and the like are used merely to a reality
Body or operation are distinguished with another entity or operation, are deposited without necessarily requiring or implying between these entities or operation
In any actual relationship or order or sequence.Moreover, the terms "include", "comprise" or its any other variant are intended to
Non-exclusive inclusion, so that the process, method, article or equipment including a series of elements is not only wanted including those
Element, but also including other elements that are not explicitly listed, or further include for this process, method, article or equipment
Intrinsic element.In the absence of more restrictions, the element limited by sentence "including a ...", it is not excluded that
There is also other identical elements in process, method, article or equipment including the element.
Each embodiment in this specification is all made of relevant mode and describes, same and similar portion between each embodiment
Dividing may refer to each other, and each embodiment focuses on the differences from other embodiments.Especially for system reality
For applying example, since it is substantially similar to the method embodiment, so being described relatively simple, related place is referring to embodiment of the method
Part explanation.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the scope of the present invention.It is all
Any modification, equivalent replacement, improvement and so within the spirit and principles in the present invention, are all contained in protection scope of the present invention
It is interior.
Claims (9)
1. whether a kind of determining psoralea corylifolia passes through the method for frying, which is characterized in that the described method includes:
(1) Malaytea Scurfpea Fruit that quality is M1 is weighed, is extracted with the low concentration alcohol that volume is V1, it is molten to obtain the first test sample
Liquid, measure Psoralenoside, the concentration of psoralen or Isopsoralenoside in first test solution, Isopsoralen it is dense
Degree；
The Malaytea Scurfpea Fruit that quality is M2 is weighed, the high concentration alcohol for being V2 with volume extracts, the second test solution is obtained,
Measure the concentration of Psoralenoside, the concentration of psoralen or Isopsoralenoside, Isopsoralen in second test solution；
Wherein, M2:V2=M1:V1, the high concentration alcohol are the alcohol of concentration of volume percent >=75%, the pure and mild institute of high concentration
State difference >=25% of the percent concentration of low concentration alcohol；
(2) Psoralenoside is calculated in the ratio of concentration and the concentration in the second test solution in the first test solution
S1, and psoralen is calculated in the ratio S2 of concentration and the concentration in the second test solution in the first test solution；
In the case where 0.9≤S1≤1.1 and S2≤1.1, determine the psoralea corylifolia by frying；
Or
Isopsoralenoside is calculated in the ratio T1 of concentration and concentration in the second test solution in the first test solution,
And Isopsoralen is calculated in the ratio T2 of concentration and the concentration in the second test solution in the first test solution；
In the case where 0.9≤T1≤1.1 and T2≤1.1, determine the psoralea corylifolia by frying；
Wherein, M1:V1 is 1mg/mL~20mg/mL；The concentration of volume percent of the low concentration alcohol is more than or equal to 50%.
2. the method as described in claim 1, which is characterized in that the alcohol is at least one of methanol, ethyl alcohol.
3. the method as described in claim 1, which is characterized in that the low concentration alcohol is concentration of volume percent≤60%
Alcohol.
4. method as claimed in claim 3, which is characterized in that the low concentration alcohol is that concentration of volume percent is 50%
Alcohol.
5. the method as described in claim 1, which is characterized in that it is 100% that the high concentration alcohol, which is concentration of volume percent,
Alcohol.
6. the method as described in claim 1, which is characterized in that in step (1), measured using ultra performance liquid chromatography described in
Psoralenoside, the concentration of psoralen or Isopsoralenoside, different benefit in first test solution and second test solution
The concentration of bone fat element.
7. method as claimed in claim 6, which is characterized in that the default chromatographic condition of ultra performance liquid chromatography includes:
Chromatographic column: using the stationary phase of octadecylsilane chemically bonded silica；Mobile phase: A phase is that 0.01%~1% formic acid is water-soluble
Liquid, B phase are methanol；Gradient elution, the gradient elution specifically: methanol accounts for the percent by volume of mobile phase in following ranges
Increase as time increases, 0 minute~6 minutes, 10%~60%.
8. the method for claim 7, which is characterized in that the default chromatographic condition of ultra performance liquid chromatography further include:
Column temperature: 50 DEG C~70 DEG C；Flow velocity: 0.1mL/ minutes~0.5mL/ minutes；Detection wavelength: 246nm~254nm；Sample volume:
1 μ of μ L~5 L.
9. such as method described in any item of the claim 1 to 8, which is characterized in that described to be extracted as ultrasonic extraction, refluxing extraction
At least one of.
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