CN108680664A - A kind of method of quick measurement Nuciferine purity - Google Patents
A kind of method of quick measurement Nuciferine purity Download PDFInfo
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Abstract
The present invention provides a kind of methods of quick measurement Nuciferine purity, belong to compound purity determination techniques field, more particularly to a kind of method measuring Nuciferine purity.Include the following steps：Obtain the purity of Nuciferine sample known at least two；Pure water Nuciferine；Nuciferine after methanol dissolving washing, ethyl acetate dissolve methanol extract, Frohde reagents are added in ethyl acetate extract, survey absorbance A under the wavelength of 410 ~ 440nm after reaction, draw the calibration curve equation of absorbance A and purity；The absorbance A for measuring unknown Nuciferine sample, brings calibration curve equation into, obtains the purity of unknown Nuciferine sample.The assay method of the present invention has the features such as accuracy is high, and assay method is simple, and cost of determination is low.
Description
Technical field
The invention belongs to compound purity determination techniques field, more particularly to a kind of method measuring Nuciferine purity.
Background technology
Nuciferine is a kind of aporphine alkaloids in lotus leaf, is the main Lipid-lowering activities ingredient in lotus leaf；To dry
The lotus leaf of crushing is raw material, a series of using cellulase pretreatment, dilute hydrochloric acid extraction, the extraction of ultrasonic wave assisted extraction, chloroform
Method is extracted.The wherein lotus leaf highest containing Nuciferine in Jiangxi Shicheng producing region.
Wang Yuxia etc. studies lotus leaf alkaloid extraction and purification process, is carried with further carrying out lotus leaf alkaloid in a deep going way
Object pharmacological activity and pharmacokinetic in vivo are taken, while being established for its large-scale industrial production and clinical application
Basis.Method using acid-dye colorimetry and high performance liquid chromatography measure respectively total alkaloid of lotus leaves and leading indicator at
The content for dividing 2-hydroxy-1-methoxy-aporphine, Nuciferine, using the preferred lotus leaf alkaloid optimum extraction work of orthogonal design method
Then skill investigates the technique using cation exchange resin purifying lotus leaf alkaloid.As a result the optimum extraction work of lotus leaf alkaloid
Skill is 16 times of medicinal material, 90% ethyl alcohol of amount extraction 3 times, every time 1.5 h;The best purifying process of lotus leaf alkaloid is lotus leaf medicinal material 90%
Ethanol extract, is recovered under reduced pressure solvent, and 20 times of amount mass fractions of residue dosing material are centrifugation after 1%HCl ultrasonic disperses, supernatant
Liquid stream with 50% ethyl alcohol, 5 times of column volume (BV) elution removal of impurities, then uses mass fraction through D001-CC large hole cation exchanger resin columns
It is 70% elution, 7 BV, 10 BV/h of elution flow rate for concentration of alcohol in 1% ammonia ethanol water wherein ethanol water, receives
Collect ammonia ethanol eluate, solvent is recovered under reduced pressure, residue is dried under reduced pressure, and obtains lotus leaf alkaloid position.Conclusion this method technique
Relatively simple, at low cost, environmental pollution is small, and lotus leaf alkaloid position obtained total alkaloid content is 50% or more.
Mostly use macroreticular resin purifying lotus leaf total alkali greatly at present, and Nuciferine purity detecting is to isolate and purify
Most time-consuming thing in the process, generally use HPLC methods are measured standard specimen, then using comparison, calculate peak area and survey
Determine the purity of Nuciferine, not only of high cost but also time-consuming and laborious, the determination efficiency substantially reduced, thus inventor be found that
A kind of simple method for measuring Nuciferine purity, can quickly measure the purity of Nuciferine, greatly improve conventional efficient.
Invention content
More in order to solve Nuciferine purity testing step, HPLC methods cost of determination is high, to instrument requirements also high present situation, this
Invention proposes a kind of method of quick measurement Nuciferine purity, and the method for measuring Nuciferine purity includes the following steps：
1. obtaining the purity of Nuciferine sample known at least two；
2. accurately weighing Nuciferine sample, impregnated with level-one pure water, then with level-one pure water, the Nuciferine sample after being washed
Product, and dry, the Nuciferine after being washed；
3. the Nuciferine after methanol dissolving washing, uses filter-cloth filtering, takes filtrate, and it is molten to remove methanol therein after being completely dissolved
Agent obtains methanol extract；
4. ethyl acetate dissolves methanol extract, filter-cloth filtering is used after being completely dissolved, takes filtrate, and remove ethyl acetate therein
Solvent obtains ethyl acetate extract；
5. Frohde reagents are added in ethyl acetate extract, Frohde reagent reaction solutions are obtained, Frohde reagent reaction solutions are taken,
According to 1:4~1:8 ratio is added 0.8 ~ 2% NaOH solution, shaken well, keeps the temperature 5 ~ 20min under conditions of 50 ~ 65 DEG C, takes
Go out 5 ~ 20min of water cooling, surveys absorbance under the wavelength of 410 ~ 440nm, obtain absorbance A；
6. drawing the calibration curve equation of absorbance A and purity according to the absorbance A of at least two Nuciferine samples and purity；
7. according to step 2. ~ 5. measure the absorbance A of unknown Nuciferine sample, substitute into the calibration curve equation of step 6., obtain
The purity of unknown Nuciferine sample.
Wherein, the purity of Nuciferine sample is calibrated using HPLC.
Further, the aperture of the filter cloth is 50 ~ 500 μm.
Further, the pure water soaking time is 2 ~ 3h.
Further, the removal methanol solvate therein is specifically by filtrate at 30 ~ 60 DEG C, under conditions of 0.1 ~ 0.6MPa
Rotary evaporation removes methanol solvate.
Further, removal ethyl acetate solvent therein is specifically by filtrate at 50 ~ 80 DEG C, the item of 0.1 ~ 0.5MPa
Evaporative removal ethyl acetate solvent is rotated under part.
Further, the step 5. described in Frohde reagents be 1% sodium molybdate concentrated sulfuric acid solution.
Advantageous effect
Applicant has found in an experiment, and lotus leaf can be substantially completely removed by washing, methanol extraction and ethyl acetate extraction
Interference impurity in alkali sample, ethyl acetate extract with Frohde reagents（The concentrated sulfuric acid solution of 1% sodium molybdate）After reaction,
Its shade has that linear positive is related to the purity of Nuciferine sample, if directly using Nuciferine example reaction, obtains not
It is linear positive correlation curve, and obtained Frohde reagent reaction solutions needs mix shaken well with NaOH solution, then 50 ~
5 ~ 20min is kept the temperature under conditions of 65 DEG C, takes out the linear correlation of ability after 5 ~ 20min of water cooling.Linear equation under other conditions
R2Respectively less than 0.99, can not Accurate Determining Nuciferine sample purity.
The method that the present invention measures Nuciferine sample purity is simple, and cost of determination is low, if condition is identical, standard curve
It can be used repeatedly for formula, greatly reduces experiment labor intensity and quantity, in various Nuciferine determination experiments room and can determine
Examination enterprise is measured to promote the use of.
Description of the drawings
Fig. 1：Nuciferine standard specimen HPLC chromatogram
Fig. 2：The linear relationship chart of Nuciferine purity and absorbance A in embodiment 1
Fig. 3：The linear relationship chart for the Nuciferine purity and absorbance A that HPLC is measured in embodiment 1
Fig. 4：The linear relationship chart of Nuciferine purity and absorbance A in embodiment 2
Fig. 5：The linear relationship chart of Nuciferine purity and absorbance A in embodiment 3
Specific implementation mode
In the embodiment of the present invention, high performance liquid chromatograph model Eclassical W3200 (Elite), Nuciferine
Mark product are the Nuciferine mark product of the Shanghai bio tech ltd Qi Ming, and high-purity Nuciferine is bought from the special biological section of Shaanxi Fes
Skill Co., Ltd.
Other chemical reagent used in the embodiment of the present invention are that analysis is pure.
Embodiment 1
A kind of method of quick measurement Nuciferine purity is present embodiments provided, concrete operation method is as follows：
1,50.00mg Nuciferine samples accurately are weighed, is settled to 10mL with level-one pure water, and stand 2 ~ 3h, obtains mixed liquor I.
2, after filtering mixed liquor I, then with level-one pure water 2 ~ 3 times, the Nuciferine sample after being washed is placed in
It is dried under conditions of 105 DEG C, the Nuciferine after being washed.
3, it with the Nuciferine after the dissolving washing of 10mL methanol, fully vibrates, and use aperture for 100 μm of filter-cloth filtering,
Filtrate is taken, by filtrate at 40 DEG C, rotary evaporation removes methanol solvate under conditions of 0.2MPa, obtains methanol extract.
4, methanol extract is dissolved with 10mL ethyl acetate, fully vibrates, and use aperture for 100 μm of filter-cloth filtering, takes
Filtrate, by filtrate at 70 DEG C, rotary evaporation removes ethyl acetate solvent under conditions of 0.2MPa, obtains ethyl acetate extract.
5, the Frohde reagents of 10mL are added in ethyl acetate extract（The concentrated sulfuric acid solution of 1% sodium molybdate）, obtain
Frohde reagent reaction solutions take the above-mentioned solution of 0.5 mL to have in plug scale colorimetric cylinder in 10 mL, add 4.5 mL's 1.5%
NaOH solution, shaken well keep the temperature 10min under conditions of 50 DEG C, take out water cooling 5min, absorbance is surveyed under the wavelength of 425nm,
Absorbance A is obtained, absorbance A is proportionate with Nuciferine sample purity.
The known Nuciferine sample for taking 10%, 20%, 50%, 60%, 70%, 80% and 90% respectively, measures in aforementioned manners respectively
Absorbance A, result is as follows, and the standard curve that thus data obtain is shown in Fig. 2, is learnt by Fig. 2, R2=0.9991, meet linear pass
System can be used for being fitted the purity of Nuciferine sample.
| Sample | 10% | 20% | 50% | 60% | 70% | 80% | 90% |
| Absorbance | 0.152 | 0.327 | 0.808 | 0.923 | 1.086 | 1.211 | 1.305 |
In order to verify accuracy, and the lotus leaf alkali content in Nuciferine sample is measured with the method for HPLC, result is as follows
Table, the standard curve that thus data obtain are shown in Fig. 3, are learnt by Fig. 3, R2=0.9995, meet linear relationship, can use formula y=
1.4821x+0.0295 the purity of the Nuciferine sample to be fitted HPLC measurement.
| Sample | 10% | 20% | 50% | 60% | 70% | 80% | 90% |
| The lotus leaf alkali content that HPLC is measured | 9.6161% | 20.0074% | 49.9976% | 60.0127% | 70.3188% | 80.0018% | 89.7418% |
The Nuciferine sample that a unknown purity is measured according to step 1 ~ 5, obtains absorbance A, carry it into formula y=
1.4821x+0.0295, you can obtain the purity of Nuciferine sample, wherein y is absorbance A, and x is purity.
For example it is 0.812 to measure the absorbance A of Nuciferine sample, and it can be by calculating, purity 52.7967%.
Embodiment 2
A kind of method of quick measurement Nuciferine purity is present embodiments provided, concrete operation method is as follows：
1,30.00mg Nuciferine samples accurately are weighed, is settled to 10mL with level-one pure water, and stand 2 ~ 3h, obtains mixed liquor I.
2, after filtering mixed liquor I, then with level-one pure water 2 ~ 3 times, the Nuciferine sample after being washed is placed in
10min is dried under conditions of 105 DEG C, the Nuciferine after being washed.
3, it with the Nuciferine after the dissolving washing of 50mL methanol, fully vibrates, and use aperture for 500 μm of filter-cloth filtering,
Filtrate is taken, by filtrate at 30 DEG C, rotary evaporation removes methanol solvate under conditions of 0.1MPa, obtains methanol extract.
4, methanol extract is dissolved with 10mL ethyl acetate, fully vibrates, and use aperture for 500 μm of filter-cloth filtering, takes
Filtrate, by filtrate at 50 DEG C, rotary evaporation removes ethyl acetate solvent under conditions of 0.1MPa, obtains ethyl acetate extract.
5, the Frohde reagents of 20mL are added in ethyl acetate extract（The concentrated sulfuric acid solution of 1% sodium molybdate）, obtain
Frohde reagent reaction solutions take the above-mentioned solution of 1 mL to have in plug scale colorimetric cylinder in 10 mL, and the NaOH for adding 6 mL 1% is molten
Liquid, shaken well keep the temperature 20min under conditions of 60 ± 5 DEG C, take out water cooling 20min, survey absorbance under the wavelength of 410nm, obtain
To absorbance A, absorbance A is proportionate with Nuciferine sample purity.
The known Nuciferine sample for taking 10%, 20%, 50%, 60%, 70%, 80% and 90% respectively, measures in aforementioned manners respectively
Absorbance A, result are as follows：
| Sample | 10% | 20% | 50% | 60% | 70% | 80% | 90% |
| Absorbance | 0.152 | 0.327 | 0.808 | 0.923 | 1.086 | 1.211 | 1.305 |
The Nuciferine sample that a unknown purity is measured according to step 1 ~ 5, obtains absorbance A, carry it into formula y=
0.9956x-0.0055, you can obtain the purity of Nuciferine sample, wherein y is absorbance A, and x is purity.
Embodiment 3
A kind of method of quick measurement Nuciferine purity is present embodiments provided, concrete operation method is as follows：
1,100.00mg Nuciferine samples accurately are weighed, is settled to 25mL with level-one pure water, and stand 2 ~ 3h, obtains mixed liquor I.
2, after filtering mixed liquor I, then with level-one pure water 2 ~ 3 times, the Nuciferine sample after being washed is placed in
10min is dried under conditions of 105 ± 5 DEG C, the Nuciferine after being washed.
3, it with the Nuciferine after the dissolving washing of 100mL methanol, fully vibrates, and use aperture for 50 μm of filter-cloth filtering,
Filtrate is taken, by filtrate at 60 DEG C, rotary evaporation removes methanol solvate under conditions of 0.6MPa, obtains methanol extract.
4, methanol extract is dissolved with 10mL ethyl acetate, fully vibrates, and use aperture for 500 μm of filter-cloth filtering, takes
Filtrate, by filtrate at 80 DEG C, rotary evaporation removes ethyl acetate solvent under conditions of 0.5MPa, obtains ethyl acetate extract.
5, the Frohde reagents of 50mL are added in ethyl acetate extract（The concentrated sulfuric acid solution of 1% sodium molybdate）, obtain
Frohde reagent reaction solutions take the above-mentioned solution of 1mL to have in plug scale colorimetric cylinder in 10 mL, and the NaOH for adding 8mL 0.8% is molten
Liquid, shaken well keep the temperature 5min under conditions of 60 DEG C, take out water cooling 10min, survey absorbance under the wavelength of 440nm, inhaled
Luminosity A, absorbance A are proportionate with Nuciferine sample purity.
The known Nuciferine sample for taking 10%, 20%, 50%, 60%, 70%, 80% and 90% respectively, measures in aforementioned manners respectively
Absorbance A, result are as follows：
| Sample purity | 10% | 20% | 50% | 60% | 70% | 80% | 90% |
| Absorbance A | 0.189 | 0.381 | 0.981 | 1.155 | 1.318 | 1.51 | 1.667 |
The Nuciferine sample that a unknown purity is measured according to step 1 ~ 5, obtains absorbance A, carries it into formula y=1.8624x
+ 0.0177, you can obtain the purity of Nuciferine sample, wherein y is absorbance A, and x is purity.
Claims (7)
1. a kind of method of quick measurement Nuciferine purity, which is characterized in that the method for measuring Nuciferine purity includes such as
Lower step：
Obtain the purity of Nuciferine sample known at least two；
Nuciferine sample accurately is weighed, is impregnated with level-one pure water, then with level-one pure water, the Nuciferine sample after being washed
Product, and dry, the Nuciferine after being washed；
Nuciferine after methanol dissolving washing, uses filter-cloth filtering, takes filtrate, and it is molten to remove methanol therein after being completely dissolved
Agent obtains methanol extract；
Ethyl acetate dissolves methanol extract, and filter-cloth filtering is used after being completely dissolved, takes filtrate, and it is molten to remove ethyl acetate therein
Agent obtains ethyl acetate extract；
Frohde reagents are added in ethyl acetate extract, obtains Frohde reagent reaction solutions, takes Frohde reagent reaction solutions, press
According to 1:4~1:8 ratio is added 0.8 ~ 2% NaOH solution, shaken well, keeps the temperature 5 ~ 20min under conditions of 50 ~ 65 DEG C, takes out
5 ~ 20min of water cooling surveys absorbance under the wavelength of 410 ~ 440nm, obtains absorbance A；
The calibration curve equation of absorbance A and purity is drawn according to the absorbance A of at least two Nuciferine samples and purity；
According to step 2. ~ 5. measure the absorbance A of unknown Nuciferine sample, substitute into the calibration curve equation of step 6., obtain not
Know the purity of Nuciferine sample.
2. the method for quick measurement Nuciferine purity according to claim 1, which is characterized in that step 1. in use HPLC
Calibrate the purity of the known Nuciferine sample.
3. the method for quick measurement Nuciferine purity according to claim 1, which is characterized in that the aperture of the filter cloth is
50~500μm。
4. the method for quick measurement Nuciferine purity according to claim 1, which is characterized in that the pure water soaking time
For 2 ~ 3h.
5. the method for quick measurement Nuciferine purity according to claim 1, which is characterized in that the removal first therein
Alcoholic solvent is specifically by filtrate at 30 ~ 60 DEG C, and rotary evaporation removes methanol solvate under conditions of 0.1 ~ 0.6MPa.
6. the method for quick measurement Nuciferine purity according to claim 1, which is characterized in that the removal second therein
Acetoacetic ester solvent is specifically by filtrate at 50 ~ 80 DEG C, and rotary evaporation removes ethyl acetate solvent under conditions of 0.1 ~ 0.5MPa.
7. the method for quick measurement Nuciferine purity according to claim 1, which is characterized in that the step 5. described in
Frohde reagents are the concentrated sulfuric acid solution of 1% sodium molybdate.
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