CN111351883B - Method for measuring rutin content in Sophora japonica and radix scutellariae ointment - Google Patents
Method for measuring rutin content in Sophora japonica and radix scutellariae ointment Download PDFInfo
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- JMGZEFIQIZZSBH-UHFFFAOYSA-N Bioquercetin Natural products CC1OC(OCC(O)C2OC(OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5)C(O)C2O)C(O)C(O)C1O JMGZEFIQIZZSBH-UHFFFAOYSA-N 0.000 title claims abstract description 70
- IVTMALDHFAHOGL-UHFFFAOYSA-N eriodictyol 7-O-rutinoside Natural products OC1C(O)C(O)C(C)OC1OCC1C(O)C(O)C(O)C(OC=2C=C3C(C(C(O)=C(O3)C=3C=C(O)C(O)=CC=3)=O)=C(O)C=2)O1 IVTMALDHFAHOGL-UHFFFAOYSA-N 0.000 title claims abstract description 70
- FDRQPMVGJOQVTL-UHFFFAOYSA-N quercetin rutinoside Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 FDRQPMVGJOQVTL-UHFFFAOYSA-N 0.000 title claims abstract description 70
- IKGXIBQEEMLURG-BKUODXTLSA-N rutin Chemical compound O[C@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@@H]1OC[C@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 IKGXIBQEEMLURG-BKUODXTLSA-N 0.000 title claims abstract description 70
- ALABRVAAKCSLSC-UHFFFAOYSA-N rutin Natural products CC1OC(OCC2OC(O)C(O)C(O)C2O)C(O)C(O)C1OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5 ALABRVAAKCSLSC-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 235000005493 rutin Nutrition 0.000 title claims abstract description 70
- 229960004555 rutoside Drugs 0.000 title claims abstract description 70
- 239000002674 ointment Substances 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 24
- 244000046101 Sophora japonica Species 0.000 title claims description 19
- 235000010586 Sophora japonica Nutrition 0.000 title claims description 19
- 239000012488 sample solution Substances 0.000 claims abstract description 41
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 174
- 238000005303 weighing Methods 0.000 claims description 78
- 239000000243 solution Substances 0.000 claims description 66
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 32
- 238000001914 filtration Methods 0.000 claims description 29
- 238000012360 testing method Methods 0.000 claims description 29
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 24
- 238000009210 therapy by ultrasound Methods 0.000 claims description 24
- 239000013558 reference substance Substances 0.000 claims description 23
- 239000000706 filtrate Substances 0.000 claims description 19
- 238000001816 cooling Methods 0.000 claims description 18
- 239000012528 membrane Substances 0.000 claims description 17
- 239000007788 liquid Substances 0.000 claims description 16
- 230000001502 supplementing effect Effects 0.000 claims description 16
- 238000000227 grinding Methods 0.000 claims description 14
- 238000005259 measurement Methods 0.000 claims description 13
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 12
- 238000001514 detection method Methods 0.000 claims description 8
- 239000000945 filler Substances 0.000 claims description 6
- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 claims description 6
- 239000012088 reference solution Substances 0.000 claims description 6
- 239000000377 silicon dioxide Substances 0.000 claims description 6
- 241000207929 Scutellaria Species 0.000 claims description 3
- 239000012982 microporous membrane Substances 0.000 claims description 3
- 239000010404 Scutellaria baicalensis extract Substances 0.000 claims 1
- 239000011148 porous material Substances 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 26
- 239000003814 drug Substances 0.000 abstract description 7
- 229940079593 drug Drugs 0.000 abstract description 4
- 238000004128 high performance liquid chromatography Methods 0.000 abstract description 3
- 239000000523 sample Substances 0.000 description 27
- 239000000203 mixture Substances 0.000 description 12
- 238000001704 evaporation Methods 0.000 description 10
- 238000000605 extraction Methods 0.000 description 9
- 238000011835 investigation Methods 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 241000219784 Sophora Species 0.000 description 6
- 238000007865 diluting Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 238000011084 recovery Methods 0.000 description 5
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 4
- 235000013399 edible fruits Nutrition 0.000 description 4
- 238000005070 sampling Methods 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000013642 negative control Substances 0.000 description 3
- 239000003208 petroleum Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000006228 supernatant Substances 0.000 description 3
- 238000012795 verification Methods 0.000 description 3
- 235000014459 Sorbus Nutrition 0.000 description 2
- 241001092391 Sorbus Species 0.000 description 2
- 229960000583 acetic acid Drugs 0.000 description 2
- 239000012362 glacial acetic acid Substances 0.000 description 2
- 208000014617 hemorrhoid Diseases 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000011550 stock solution Substances 0.000 description 2
- 239000012085 test solution Substances 0.000 description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 2
- 241001251200 Agelas Species 0.000 description 1
- 241000382455 Angelica sinensis Species 0.000 description 1
- 208000012671 Gastrointestinal haemorrhages Diseases 0.000 description 1
- 238000010268 HPLC based assay Methods 0.000 description 1
- 208000032843 Hemorrhage Diseases 0.000 description 1
- 235000003417 Plumeria rubra f acutifolia Nutrition 0.000 description 1
- 244000040691 Plumeria rubra f. acutifolia Species 0.000 description 1
- 208000012287 Prolapse Diseases 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000740 bleeding effect Effects 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 208000035861 hematochezia Diseases 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 201000007772 internal hemorrhoid Diseases 0.000 description 1
- 238000012417 linear regression Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 208000011580 syndromic disease Diseases 0.000 description 1
- 238000011003 system suitability test Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 238000002137 ultrasound extraction Methods 0.000 description 1
- 238000010200 validation analysis Methods 0.000 description 1
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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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
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- General Physics & Mathematics (AREA)
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Abstract
The invention belongs to the technical field of medicines, and particularly relates to a method for measuring the content of rutin in a sophorae radix ointment. The rutin content determination method is high performance liquid chromatography. The rutin content determination method simplifies the preparation method of the sample solution, simplifies the experimental operation and improves the experimental efficiency.
Description
Technical Field
The invention belongs to the technical field of medicines, and particularly relates to a method for measuring the content of rutin in a sophorae radix ointment.
Background
The Sophora japonica and radix scutellariae ointment is an exclusive variety of Daqian prescription pharmaceutical limited company in Shandong, is composed of eight medicinal materials of Sophora japonica, radix paeoniae rubra, moutan bark, angelica sinensis, radix sileris, fructus aurantii, radix scutellariae and radix aconiti preparata, and has the effects of clearing heat, stopping bleeding, and relieving swelling and pain. Can be used for treating internal hemorrhoid of stage I and II or mixed hemorrhoid with syndrome of downward flow of damp-heat of stage I and II, manifested by hematochezia, pain, local discomfort, and hemorrhoid prolapse. At present, the standard is an internal control standard of a company, and no public quality standard is found.
Rutin is the main active ingredient of the traditional Chinese medicine sophora fruit, and the feeding condition of the sophora fruit medicinal material can be reflected by the content measurement of rutin, thereby being beneficial to the quality control of sophora fruit ointment finished products.
The original internal control standard content determination method of the sophorae and scutellaria ointment comprises the following steps:
octadecylsilane chemically bonded silica is used as a filler for chromatographic conditions and system suitability test: tetrahydrofuran-water-glacial acetic acid (22:78:2) as mobile phase: the detection wavelength was 359nm. The theoretical plate number is not lower than 1000 according to rutin peak.
The preparation of the control solution precisely weighs a proper amount of rutin control substance which is dried to constant weight under reduced pressure at 120 ℃, methanol is added to prepare 20 mug solution per 1ml, and the solution is uniformly shaken to obtain the rutin control solution.
Preparing a sample solution, namely taking about 1g of Sophora baicalensis ointment, precisely weighing, placing the Sophora baicalensis ointment into a conical bottle with a plug, adding 50ml of ethanol, carrying out ultrasonic treatment (power is 250W, frequency is 20 kHz) for 20 minutes, evaporating the solution to a small volume in a water bath, adding 2.5g of diatomite, uniformly stirring the solution, evaporating the solution to dryness, adding 50ml of petroleum ether (60-90 ℃) and ultrasonic treatment (power is 250W, frequency is 20 kHz) for 20 minutes, cooling the solution, pouring out the supernatant, evaporating the residue in a water bath at 80 ℃, precisely adding 50ml of methanol, weighing the solution, carrying out ultrasonic treatment (power is 250W, frequency is 20 kHz) for 20 minutes, cooling the solution, weighing the solution again, supplementing the reduced weight with methanol, shaking the solution, filtering the filtrate, and filtering the filtrate with a microporous filter membrane (0.45 mu m).
And respectively precisely sucking 20 mu l of the reference substance solution and 20 mu l of the sample solution by the measuring method, injecting into a liquid chromatograph, and measuring to obtain the liquid chromatograph.
The ointment contains fructus Sophorae (parched) and rutin (C) per lg 27 H 30 O 16 ) And not less than 1.1mg.
The above measurement method has the following problems:
(1) because the sophorae and scutellaria ointment is an ointment, the ointment contains more grease components, the extraction effect can be affected by directly extracting with methanol, and the extracting solution contains a large amount of fat-soluble matrixes to pollute a chromatographic system.
(2) The solubility of rutin in pure methanol is superior to other extraction solvents, and if heating extraction is adopted, more fat-soluble matrix is brought to the sample solution, and the chromatographic system is seriously polluted.
(3) The preparation method of the sample solution in the original standard comprises the steps of taking about 1g of sophoro ointment, precisely weighing, placing the sophoro ointment into a conical bottle with a plug, adding 50ml of ethanol, carrying out ultrasonic treatment (with the power of 250W and the frequency of 20 KHZ) for 20 minutes, evaporating the mixture to a small volume in a water bath, adding 2.5g of diatomite, uniformly stirring the mixture, evaporating the mixture to dryness, adding 50ml of petroleum ether (with the power of 60-90 ℃) for 50 minutes, carrying out ultrasonic treatment (with the power of 250W and the frequency of 20 KHZ) for 20 minutes, cooling the mixture, pouring out supernatant, evaporating the residue in a water bath at the temperature of 80 ℃, precisely adding 50ml of methanol, weighing, carrying out ultrasonic treatment for 20 minutes, cooling the mixture, weighing again, supplementing the reduced weight with methanol, shaking the mixture, filtering the mixture, and filtering the subsequent filtrate with a microporous filter membrane (0.45 mu m), thus obtaining the product with complex operation and low test efficiency.
(4) The chromatographic purity of tetrahydrofuran in the mobile phase in chromatographic conditions is not usual in the laboratory and is relatively damaging to the chromatographic system.
Disclosure of Invention
In order to solve the technical problems, the invention provides a method for measuring the content of rutin in a sophorae radix ointment.
The invention solves the technical problems by the following technical proposal
A method for measuring rutin content in Sophora japonica and radix Scutellariae ointment comprises high performance liquid chromatography.
The method for measuring the rutin content in the sophorae radix ointment comprises the following chromatographic conditions: octadecylsilane chemically bonded silica is used as a filler; methanol-acetonitrile-0.5% phosphoric acid solution (13:13:74) as mobile phase; the flow rate was 1.0mL/min, the column temperature was 30deg.C, and the detection wavelength was 359nm. The volume ratio of the methanol-acetonitrile-0.5% phosphoric acid solution is 13:13:74.
In the method for measuring the content of rutin,
preparing a sample solution, namely, taking 3g of sophora japonica ointment, precisely weighing, adding 2 times of diatomite, precisely weighing, grinding, taking 1g, precisely weighing, placing in a conical bottle with a plug, precisely adding 25ml of methanol, weighing, performing ultrasonic treatment for 30 minutes, cooling, weighing again, supplementing the lost weight with methanol, shaking uniformly, filtering, and taking a subsequent filtrate to filter with a microporous membrane.
In the method for measuring the rutin content in the sophorae radix ointment, the ultrasonic power of ultrasonic treatment is 250W, and the frequency is 20kHz. The aperture of the microporous filter membrane is 0.45 mu m.
The method for measuring the rutin content in the sophorae radix ointment comprises the following steps:
octadecylsilane chemically bonded silica is used as a filler for chromatographic conditions and system applicability tests; methanol-acetonitrile-0.5% phosphoric acid solution (13:13:74) as mobile phase; the flow rate was 1.0mL/min, the column temperature was 30deg.C, and the detection wavelength was 359nm. The number of theoretical plates is not lower than 2500 according to rutin peaks;
preparing a reference substance solution, namely taking a proper amount of rutin reference substance, precisely weighing, and adding methanol to prepare a solution containing 40 mu g of each 1ml of the solution;
preparing a sample solution, namely, taking 3g of sophora japonica ointment, precisely weighing, adding 2 times of diatomite, precisely weighing, grinding, taking about 1g, precisely weighing, placing in a conical bottle with a plug, precisely adding 25ml of methanol, weighing, performing ultrasonic treatment (with the power of 250W and the frequency of 20 kHz) for 30 minutes, cooling, weighing again, supplementing the lost weight with methanol, shaking uniformly, filtering, and taking a subsequent filtrate, and filtering with a microporous filter membrane (0.45 mu m);
and respectively precisely sucking 10 mu l of the reference substance solution and 10 mu l of the sample solution by the measuring method, injecting into a liquid chromatograph, and measuring to obtain the liquid chromatograph.
The 0.5% phosphoric acid solution is a phosphoric acid solution with the mass percentage concentration of 0.5%.
The invention has the advantages that,
(1) the diatomite is used for adsorbing oil and fat components in the preparation of the sample solution, and then methanol is used for extraction, so that the extraction effect is better, the phenomenon that more oil and fat components in the Sophora japonica and radix scutellariae ointment affect the extraction of rutin is avoided, and meanwhile, the fact that the extracting solution contains a large amount of fat-soluble matrixes and pollutes a chromatographic system is avoided.
(2) The solubility of rutin in pure methanol is superior to other extraction solvents, if the heating extraction is adopted, more fat-soluble matrixes are brought to the sample solution, and the chromatographic system is seriously polluted, so the water bath evaporation step is omitted in the extraction method, and the damage of the chromatographic system caused by the heating of more fat-soluble matrixes brought to the sample solution is avoided.
(3) The preparation method of the sample solution is simplified, the original standard of taking about 1g of the sophorae radix ointment, precisely weighing, placing the sophorae radix ointment into a conical bottle with a plug, adding 50ml of ethanol, carrying out ultrasonic treatment (with the power of 250W and the frequency of 20 KHZ) for 20 minutes, evaporating the mixture to a small volume in a water bath, adding 2.5g of diatomite, uniformly stirring, evaporating the mixture to dryness, adding 50ml of petroleum ether (with the power of 60-90 ℃) for 50 minutes, carrying out ultrasonic treatment (with the power of 250W and the frequency of 20 KHZ) for 20 minutes, cooling, pouring out supernatant, evaporating the residue in a water bath at the temperature of 80 ℃, precisely adding 50ml of methanol, weighing, carrying out ultrasonic treatment for 20 minutes, cooling, weighing again, supplementing the lost weight with methanol, shaking, filtering, taking the subsequent filtrate, filtering with a microporous filter membrane (with the frequency of 0.45 mu m), obtaining the modified ointment, adding twice amount of diatomite, grinding the diatomite, directly adding methanol for ultrasonic extraction, simplifying experimental operation, and improving experimental efficiency.
(4) The chromatographic purity tetrahydrofuran in the mobile phase in the original standard chromatographic conditions is not commonly used in a laboratory and has relatively large damage to a chromatographic system, and the original standard tetrahydrofuran-water-glacial acetic acid (22:78:2) is revised to be the mobile phase methanol-acetonitrile-0.5% phosphoric acid solution (13:13:74) to be the mobile phase, so that the inspection cost is reduced and the damage to the chromatographic system is reduced.
(5) Ensuring that the rutin chromatographic peak and other impurity peaks in the sample solution have higher separation degree, and revising the theoretical plate number in the original standard to be not lower than 1000 according to the rutin peak and the theoretical plate number to be not lower than 2500 according to the rutin peak.
(6) Ensuring that the rutin chromatographic peak area of the reference substance solution has a better proportional relation with the rutin chromatographic peak area of the sample solution, precisely weighing the rutin reference substance solution prepared in the original standard, drying the rutin reference substance solution under reduced pressure at 120 ℃ until the weight is constant, adding methanol to prepare a solution containing 20 mug per 1ml, shaking the solution uniformly to obtain the rutin reference substance solution prepared in the revised mode, precisely weighing the rutin reference substance, and adding methanol to prepare a solution containing 40 mug per 1 ml.
Drawings
FIG. 1 is a diagram showing a determination test of the mobile phase for rutin content determination.
FIG. 2-A is a rutin content determination specific test chart-reference substance solution.
FIG. 2-B shows a rutin content determination specific test chart-sample solution.
FIG. 2-C shows a rutin content determination specific test chart-negative solution.
Description of the embodiments
The present invention will be further described with reference to the drawings and the detailed description, so that those skilled in the art will more readily understand the present invention, but the present invention is not limited thereto.
A method for measuring rutin content in Sophora japonica and radix Scutellariae ointment comprises the following steps:
octadecylsilane chemically bonded silica is used as a filler for chromatographic conditions and system applicability tests; methanol-ethanol-0.5% phosphoric acid solution (13:13:74) as mobile phase; the flow rate was 1.0mL/min, the column temperature was 30deg.C, and the detection wavelength was 359nm. The number of theoretical plates is not lower than 2500 according to rutin peaks;
preparing a reference substance solution, namely taking a proper amount of rutin reference substance, precisely weighing, and adding methanol to prepare a solution containing 40 mu g of each 1ml of the solution;
preparing a sample solution, namely preparing about 3g of sophorae radix ointment, precisely weighing, adding about 2 times of diatomite, precisely weighing, grinding, taking about 1g of sophorae radix ointment, precisely weighing, placing in a conical bottle with a plug, precisely adding 25ml of methanol, weighing, performing ultrasonic treatment (power is 250W and frequency is 20 kHz) for 30 minutes, cooling, weighing again, supplementing the lost weight with methanol, shaking uniformly, filtering, and filtering the subsequent filtrate with a microporous filter membrane (0.45 mu m);
and respectively precisely sucking 10 mu l of the reference substance solution and 10 mu l of the sample solution by the measuring method, injecting into a liquid chromatograph, and measuring to obtain the liquid chromatograph.
( One) HPLC assay methodological validation of rutin (sample lot number for methodological study: 19010105 )
Preparing a test solution and a reference solution of the Sophora baicalensis ointment, and testing according to the condition of the high performance liquid chromatography of the four-part rule 0512 of the 2015 edition of Chinese pharmacopoeia.
1. Verification project
a. Selecting a mobile phase; b. a chromatographic column durability test; c. examining ultrasonic time; d. investigation of the sampling quantity; e. linear relation investigation; f. performing precision test; g. repeatability investigation; h. testing the stability of a sample; i. sample addition recovery rate test; j, a specificity test; k sample assay
2. Verification implementation:
2.1 instruments and reagents
2.1.1 instruments: LC-20AT high performance liquid chromatograph; an electronic balance.
2.1.2 reagents:
methanol and acetonitrile are chromatographic pure, and other reagents are analytically pure.
2.1.3 rutin control information:
lot number: 100080-201811, content in 91.7%
The source is as follows: is provided by Chinese food and drug verification institute.
2.2 chromatography conditions and System applicability test octadecylsilane chemically bonded silica is used as filler, the detection wavelength is 359nm, methanol-acetonitrile-0.5% phosphoric acid solution (13:13:74) is used as mobile phase, the flow rate is 1.0ml/min, and the column temperature is 30 ℃; the theoretical plate number is not lower than 2500 calculated according to rutin peak.
2.2.1 screening of mobile phases
Purpose-determining common Mobile phase methanol-acetonitrile-0.5% phosphoric acid solution (13:13:74)
2.2.1.1 preparation of control solution rutin control (1) 4.185mg (2) 4.284 mg were precisely weighed, placed in 100ml measuring flask, dissolved and diluted with methanol to the scale, and shaken well to obtain (C) Pair 1 ：38.37645µg/ml、C Pair 2 ：39.37598µg/ml）。
2.2.1.2 preparation of sample solution 19010105 Sorbus ointment 3.0720g, precisely weighing, adding 6.0043g of diatomite, precisely weighing, grinding, precisely weighing the sample (1 g, 0.0132 g, (2) 0.9898g, precisely adding 25ml of methanol into a conical flask with a plug, weighing, performing ultrasonic treatment (power 250W, frequency 20 kHz) for 30 minutes, cooling, weighing again, supplementing the reduced weight with methanol, shaking, filtering, and filtering the subsequent filtrate with a microporous filter membrane (0.45 mu m).
2.2.1.3 measuring and respectively precisely sucking the reference substance solution and the sample solution by 10 mu l, and injecting into a liquid chromatograph.
2.2.1.4 conclusion: the rutin chromatographic peak in the chromatogram of the sample solution has good separation effect from other chromatographic peaks. The mobile phase was therefore determined to be methanol-acetonitrile-0.5% phosphoric acid solution (13:13:74). The results are shown in FIG. 1. FIG. 1: determining a test pattern of the mobile phase.
2.3 column durability test
Aims at examining the separation degree of rutin chromatographic peaks and other impurity peaks in the sample solutions of different chromatographic columns.
2.3.1 preparation of control solution:
2.3.1.1thermo5 [ mu ] m, 250X 4.6mmC18 chromatographic column: taking the reference substance solution of 2.2.1.1 items to obtain;
2.3.1.2Welch5 [ mu ] m, 250X 4.6mmC18 column: precisely weighing rutin control (1.340 mg, (2.4.199mg) respectively, placing into 100ml measuring flask, dissolving in methanol, diluting to scale, and shaking to obtain (C) Pair 1 ：39.7978µg/ml、C Pair 2 ：38.50483µg/ml）；
2.3.1.3Agela5 [ mu ] m, 250X 4.6mmC18 column: precisely weighing rutin control (1) 4.028mg (2) 4.161mg, respectively placing into 100ml measuring flask, dissolving in methanol, diluting to scale, and shaking to obtain (C) Pair 1 ：36.93676µg/ml、C Pair 2 ：38.15637µg/ml）。
2.3.2 preparation of test solutions:
2.3.2.1thermo5 [ mu ] m, 250X 4.6mmC18 chromatographic column: taking the sample solution under the condition of 2.2.1.2 items, and obtaining the sample solution;
2.3.2.2Welch5 [ mu ] m, 250X 4.6mmC18 column: taking 3.0384g of 19010105 sophora japonica ointment, precisely weighing, adding 6.0072g of diatomite, precisely weighing, grinding, precisely weighing a sample (1.0255 g, (2) 0.9677g, placing into a conical bottle with a plug, precisely adding 25ml of methanol, weighing, performing ultrasonic treatment (power 250W, frequency 20 kHz) for 30 minutes, cooling, weighing again, supplementing the lost weight with methanol, shaking, filtering, and filtering the subsequent filtrate with a microporous filter membrane (0.45 mu m) to obtain the medicine;
2.3.2.3Agela5 [ mu ] m, 250X 4.6mmC18 column: 19010105, 3.0528g of Sophora japonica ointment, precise weighing, 6.0176g of diatomite, precise weighing, grinding, precise weighing of a sample (1.0382 g, (2) 1.0347g, placing in a conical bottle with a plug, precisely adding 25ml of methanol, weighing, performing ultrasonic treatment (power 250W, frequency 20 kHz) for 30 minutes, cooling, weighing again, supplementing the lost weight with methanol, shaking, filtering, and filtering the subsequent filtrate with a microporous filter membrane (0.45 mu m) to obtain the product.
2.3.3 determination: respectively precisely sucking 10 μl of the above solution, injecting into liquid chromatograph, and using Thermo
5 [ mu ] m, 250X 4.6mmC18 column, welch5 [ mu ] m, 250X 4.6mmC18 column and Agela
5 [ mu ] m,250×4.6mmC18 chromatographic column, and testing according to the chromatographic conditions;
2.3.4 conclusion: the peak shape and the separation effect are ideal, and the theoretical plate numbers of the three chromatographic columns are 14449, 15048 and 14547 respectively according to rutin, and are not lower than 2500.
2.4 investigation of ultrasound time
The influence of ultrasonic time on the rutin content measurement result is examined.
2.4.1 preparation of control solution rutin control (1) 4.255 mg (2) 4.014mg, each in a 100ml measuring flask, dissolving in methanol and diluting to scale, shaking to obtain (C) Pair 1 ：39.00001µg/ml、C Pair 2 ：36.80838µg/ml）。
2.4.2 preparation of sample solution 19010105 Sorbridge ointment 2.9403g, precision weighing, adding 6.0154g of diatomite, precision weighing, grinding, precision weighing the sample (1.0207 g, (2) 1.0214g, (3) 1.0229g, (4) 1.0332g, (5) 1.0515g, (6) 1.0425g, placing into a conical flask with a plug, precision adding 25ml of methanol, weighing, ultrasonic treatment (power 250W, frequency 20 kHz) for 20 minutes, 30 minutes and 60 minutes, cooling, weighing again, supplementing the lost weight with methanol, shaking, filtering, and filtering the subsequent filtrate with microporous filter membrane (0.45 μm).
2.4.3 determination: respectively and precisely sucking 10 mu l of each solution, measuring according to the determined chromatographic conditions,
2.4.4 the results are shown in Table 1.
2.4.5 conclusion: as can be seen from the measurement results, the ultrasonic time is not different from the measurement results, various test factors are integrated, and the ultrasonic time is tentatively set for 30 minutes in order to ensure the accuracy of the measurement results.
2.5 investigation of sample size
The influence of the sampling quantity on the rutin content measurement result is examined.
2.5.1 preparation of control solution rutin control (1) 4.266mg (2) 4.073mg, respectively placing into 100ml measuring flask, dissolving in methanol, diluting to scale, and shaking to obtain (C) Pair 1 ：39.11922µg/ml、C Pair 2 ：37.34941µg/ml）。
2.5.2 preparation of sample solution the sample to be tested (1) under 2.4.2 items was precisely weighed (1) 0.5258g, (2) 0.5231g, (3) 1.0388g, (4) 1.0374g, (5) 2.0158g, (6) 2.0150g, respectively placed in conical flasks with stoppers, each of which was precisely charged with 25ml of methanol, weighed, sonicated (power 250W, frequency 20 kHz) for 30 minutes, cooled, weighed again, the reduced weight was made up with methanol, shaken well, filtered, and the subsequent filtrate was filtered with a microporous filter membrane (0.45. Mu.m), thus obtaining.
2.5.3 determination: and respectively precisely sucking 10 mu l of each solution, and measuring according to the determined chromatographic conditions, wherein the result is shown in Table 2.
2.5.4 conclusion: as is apparent from the above measurement results, there was substantially no difference in the measurement results of the three types of sampled amounts, and the sampled amount was determined to be 1.0g in consideration of errors in the sampled amount and contamination of the column.
2.6 precision test
The aim is to examine the degree of the same uniform reference substance solution between the measured results of multiple sampling under the specified test conditions, and RSD is less than or equal to 2.0 percent
2.6.1 preparation of control solution A rutin control 4.135mg was precisely weighed, placed in a 100ml measuring flask, dissolved in methanol and diluted to the scale, and shaken well to obtain (C) For a pair of ：37.91795µg/ml）。
2.6.2 determination: precisely sucking 10 mu l of reference substance solution under 2.6.1 items, injecting into a liquid chromatograph, continuously injecting sample for 6 times, and measuring the peak area. Results: see table 4.
2.6.3 conclusion: the test result shows that the instrument precision is good.
2.7 investigation of the Linear relationship
The aim is to determine whether the concentration of the sample solution and the quantitative information are in a linear relation; the linear range, i.e. the determination of the appropriate sample amount, is determined.
2.7.1 determination: precisely sucking the reference substance solutions 1, 2, 5, 10, 15 and 20 mu l under the condition of 2.6.1 respectively, injecting into a liquid chromatograph, and measuring peak areas respectively.
2.7.2 results: taking the sample injection amount of rutin reference substance as abscissa and the peak area integral value as ordinate, and performing linear regression to obtain rutin regression equation y=2×10 6 x-2516.2, correlation coefficient R 2 See table 3 for =1.
2.7.3 conclusion: the rutin sample injection quantity is in good linear relation with the peak area integral value between 0.037918 and 0.758359 mu g.
2.8 repeatability investigation
Under the same condition of target investigation, the precision of the detection result of the experimenter
2.8.1 preparation of control solution rutin control (1) (4.003mg; 2) (4.041 mg; 2) was precisely weighed, placed in 100ml measuring flask, dissolved and diluted with methanol to the scale, and shaken well to obtain (C) Pair 1 ：36.70751µg/ml、C Pair 2 ：37.05597µg/ml）。
2.8.2 preparation of sample solution the sample to be tested under 2.4.2 items (1) 1.01335 g, (2) 1.01333 g, (3) 1.0261g, (4) 1.0234g, (5) 1.0200g, (6) 1.0359g, were put into a conical flask with plug, each of which was precisely added with 25ml of methanol, weighed, sonicated (power 250W, frequency 20 kHz) for 30 minutes, cooled, weighed again, the reduced weight was complemented with methanol, shaken well, filtered, and the subsequent filtrate was filtered with a microporous filter membrane (0.45 μm), thus obtaining.
2.8.3 measuring and precisely sucking 10 mu l of a reference substance and a sample solution respectively, injecting into a liquid chromatograph, measuring and calculating the content. The results are shown in Table 5.
2.8.4 conclusion: as can be seen from the above measurement results, the reproducibility of the method was good.
2.9 sample stability test
The stability of the components to be detected in the detection process of the sample solution is inspected.
2.9.1 sample solution 1 under the repetition test 2.8.2 was taken as a sample solution.
2.9.2 determination: and sampling at intervals of 10 mu l each time, measuring the peak area of rutin, and checking for 24 hours. The results are shown in Table 6.
2.9.3 conclusion: the test result shows that the test sample solution has good stability within 24 hours, and can meet the requirement of measuring the rutin content.
2.10 sample recovery test
And (5) whether the recovery rate of the sample meets the requirement or not is inspected.
2.10.1 preparation of control solution rutin control (1) 4.050mg (2) 4.117mg, respectively placing into 100ml measuring flask, dissolving in methanol, diluting to scale, and shaking to obtain (C) Pair 1 ：37.1385µg/ml、C Pair 2 ：37.75289µg/ml）。
2.10.2 preparation of control stock solution rutin control 6.031mg is precisely weighed, placed in a 250ml measuring flask, dissolved and diluted with methanol to scale, and shaken well to obtain (C) For a pair of ：0.022122mg/ml）。
Preparation of 2.10.3 sample solution 19010105 g of Soiqin ointment 2.9728g (with known rutin content of 3.6 mg/g) is precisely weighed, 6.0045g of diatomite is added, the mixture is ground into fine powder, 0.4689g (2) 0.4655g (3) 0.4828g (4) 0.4912g (5) 0.4841g (6) 0.5131g is precisely weighed, 25ml of control stock solution is precisely added into a conical flask with a plug, the mixture is weighed, ultrasonic treatment (with power of 250W and frequency of 20 kHz) is carried out for 30 minutes, the mixture is cooled, then weighed, methanol is used for supplementing the reduced weight, shaking and filtering are carried out, and a subsequent filtrate is filtered through a microporous filter membrane (0.45 mu m).
2.10.4 measuring and precisely sucking 10 μl of the reference substance and the solution of the sample, injecting into a liquid chromatograph, measuring according to the measuring method, and calculating the recovery rate. The results are shown in Table 7.
2.10.5 conclusion: the test result shows that the sample recovery rate test of the measuring method is good.
2.11 specificity test
Objective investigation of whether auxiliary materials interfere with the measurement results
2.11.1 preparation of control solution rutin control (1) 4.096mg (2) 4.292 mg, respectively placing into 100ml measuring flask, dissolving in methanol, diluting to scale, and shaking to obtain (C) Pair 1 ：37.56032µg/ml、C Pair 2 ：39.39432µg/ml）。
2.11.2 preparation of sample solution 19010105 Sorbus ointment 3.0295g, precisely weighing, adding 6.0014g of diatomite, precisely weighing, grinding, precisely weighing sample 1.0400g, placing into a conical flask with a plug, precisely adding 25ml of methanol, weighing, performing ultrasonic treatment (power 250W, frequency 20 kHz) for 30 minutes, cooling, weighing again, supplementing the lost weight with methanol, shaking, filtering, and filtering the filtrate with microporous membrane (0.45 μm).
2.11.3 preparation of negative control solution other medicines except for the fructus Sophorae (parched) in the prescription are prepared into 3.1189g of negative sample of the fructus Sophorae (parched) according to the prescription proportion, 6.0014g of diatomite is added, grinding is carried out, 1.0055g is precisely weighed, and the negative control solution is prepared by the same preparation method of sample solution.
2.11.4 the reference solution, the sample solution and the negative reference solution are respectively sucked precisely in a measuring way of 10 mu l, and are injected into a liquid chromatograph for measuring.
2.11.5 results: the sample chromatogram has corresponding chromatographic peak at the same position with the retention time of the control chromatogram, and the negative control chromatogram has no corresponding control chromatographic peak. The patterns are shown in figures 2-A, 2-B and 2-C.
2.11.6 conclusion: the other medicinal ingredients in the prescription have no interference to the measurement result.
2.12 sample measurement
2.12.1 lot number: 18100105;190101051;190401051 Sophora japonica and radix Scutellariae ointment
Preparation of 2.12.2.1 control solution rutin control (1) 4.025mg (2) 4.107mg were precisely weighed, placed in 100ml measuring flask, dissolved and diluted with methanol to scale, and shaken well to obtain (C) Pair 1 ：36.90925µg/ml、C Pair 2 ：37.66119µg/ml）。
Preparation of 2.12.2.2 sample solution
2.12.2.2.1 precisely weighing 18100105 g of Sophora japonica and radix Scutellariae ointment 3.0839g, precisely weighing, adding 6.0678g of diatomite, precisely weighing, grinding, precisely weighing the sample (1) 0.9985g, (2) 0.9994g, placing into a conical flask with a plug, precisely adding 25ml of methanol, weighing, performing ultrasonic treatment (power 250W and frequency 20 kHz) for 30 minutes, cooling, weighing again, supplementing the reduced weight with methanol, shaking, filtering, and filtering the subsequent filtrate with a microporous filter membrane (0.45 μm).
2.12.2.2.2 precisely weighing 190101051 g of Sophora japonica and radix Scutellariae ointment 3.0295g, precisely weighing, adding 6.0014g of diatomite, precisely weighing, grinding, precisely weighing the sample (1) 0.9388g, (2) 0.9339g, placing into a conical flask with a plug, precisely adding 25ml of methanol, weighing, performing ultrasonic treatment (power 250W, frequency 20 kHz) for 30 minutes, cooling, weighing again, supplementing the reduced weight with methanol, shaking, filtering, and filtering the subsequent filtrate with microporous filter membrane (0.45 μm).
2.12.2.2.3 precisely weighing 190401051 g of Sophora japonica and radix Scutellariae ointment 3.1011g, precisely weighing, adding 6.0231g of diatomite, precisely weighing, grinding, precisely weighing the sample (1) 0.9989g, (2) 0.9783g, placing into a conical flask with a plug, precisely adding 25ml of methanol, weighing, performing ultrasonic treatment (power 250W, frequency 20 kHz) for 30 minutes, cooling, weighing again, supplementing the reduced weight with methanol, shaking, filtering, and filtering the subsequent filtrate with a microporous filter membrane (0.45 μm).
2.12.2.3 the reference solution, the sample solution and the negative reference solution are respectively sucked precisely in a measuring way of 10 mu l, and are injected into a liquid chromatograph for measuring.
2.12.3 results: see table 8.
2.12.4 conclusion: the national standard prescribes that every 1g of the Chinese medicament contains the pagodatree fruit (stir-fried) with rutin (C 27 H 30 O 16 ) And (3) measuring not less than 1.1mg, wherein the content of 3 batches of samples is in the range of 3.1-4.1 mg/g according to the revised preparation method of the sample solution.
Claims (3)
1. The method for measuring the content of rutin in the sophorae radix ointment is characterized by comprising the following steps of:
octadecylsilane chemically bonded silica is used as a filler for chromatographic conditions and system applicability tests; the methanol-acetonitrile-0.5% phosphoric acid solution is a mobile phase, and the volume ratio of the methanol-acetonitrile-0.5% phosphoric acid solution is 13:13:74; the flow rate is 1.0mL/min, the column temperature is 30 ℃, and the detection wavelength is 359nm; the number of theoretical plates is not lower than 2500 according to rutin peaks;
preparing a reference substance solution, namely adding methanol into the rutin reference substance to prepare a solution with 40 mug per 1 ml;
preparing a sample solution, namely, taking 3g of sophora japonica and scutellaria ointment, precisely weighing, adding 2 times of diatomite, precisely weighing, grinding, taking about 1g, precisely weighing, placing in a conical bottle with a plug, precisely adding 25ml of methanol, weighing, performing ultrasonic treatment for 30 minutes, cooling, weighing again, supplementing the lost weight with methanol, shaking uniformly, filtering, and taking a subsequent filtrate to filter with a microporous membrane to obtain the sophora japonica and scutellaria baicalensis extract;
respectively precisely sucking 10 μl of the reference solution and the sample solution, and injecting into a liquid chromatograph for measurement.
2. The method for measuring the rutin content in a Sophora japonica ointment according to claim 1, wherein the ultrasonic power of the ultrasonic treatment is 250W and the frequency is 20kHz.
3. The method for measuring the rutin content in a Sophora japonica ointment according to claim 1, wherein the pore size of the microporous filter membrane is 0.45 μm.
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