CN111351883A - Method for measuring content of rutin in sophora and scutellaria ointment - Google Patents
Method for measuring content of rutin in sophora and scutellaria 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 84
- 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 84
- 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 84
- 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 84
- 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 84
- 235000005493 rutin Nutrition 0.000 title claims abstract description 84
- 229960004555 rutoside Drugs 0.000 title claims abstract description 84
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- 238000001914 filtration Methods 0.000 claims description 26
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- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 13
- 239000000706 filtrate Substances 0.000 claims description 13
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- 239000012488 sample solution Substances 0.000 claims description 13
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- 238000009210 therapy by ultrasound Methods 0.000 claims description 12
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- 239000012088 reference solution Substances 0.000 claims description 8
- 239000000945 filler Substances 0.000 claims description 7
- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 claims description 7
- 239000000377 silicon dioxide Substances 0.000 claims description 7
- 230000001502 supplementing effect Effects 0.000 claims description 7
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- 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
- 241000628997 Flos Species 0.000 description 6
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- 239000000463 material Substances 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
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- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 2
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- 241001106477 Paeoniaceae Species 0.000 description 1
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- 241001180876 Saposhnikovia Species 0.000 description 1
- 240000004534 Scutellaria baicalensis Species 0.000 description 1
- 235000017089 Scutellaria baicalensis Nutrition 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
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- 230000000740 bleeding effect Effects 0.000 description 1
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- 239000013068 control sample Substances 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
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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 sophora and scutellaria ointment. The content determination method of rutin is high performance liquid chromatography. The rutin content determination method simplifies the preparation method of the test solution, simplifies the experiment operation and improves the experiment 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 sophora and scutellaria ointment.
Background
The sophora and scutellaria ointment is a unique variety of the Shandong Daqian prescription pharmaceutical Co Ltd, is composed of eight medicinal materials of sophora fruit, red paeony root, tree peony bark, Chinese angelica, divaricate saposhnikovia root, bitter orange, baical skullcap root and prepared common monkshood mother root, and has the effects of clearing heat, stopping bleeding, reducing swelling and relieving pain. Can be used for treating stage I and II internal hemorrhoid or mixed hemorrhoid complicated with stage I and II downward flow of damp-heat, with symptoms of hematochezia, pain due to tenesmus, local discomfort, and prolapse of hemorrhoid. At present, the standard is a company internal control standard, and no public quality standard exists.
Rutin is the main effective component of the traditional Chinese medicine fructus sophorae, and the feeding condition of fructus sophorae medicinal materials can be reflected through the content measurement of rutin, so that the quality control of the finished product of the fructus sophorae Qin ointment is facilitated.
The method for measuring the content of the sophora japonica-scutellaria baicalensis ointment by using the original internal control standard comprises the following steps:
chromatographic conditions and system applicability test using octadecylsilane chemically bonded silica as filler: tetrahydrofuran-water-glacial acetic acid (22:78:2) as mobile phase: the detection wavelength was 359 nm. The number of theoretical plates is not less than 1000 calculated according to rutin peak.
Preparation of control solution A proper amount of rutin control substance dried at 120 deg.C under reduced pressure to constant weight is precisely weighed, and added with methanol to obtain solution containing 20 μ g per 1ml, and shaken well to obtain the final product.
Preparing a test solution, namely taking about 1g of sophora japonica-scutellaria ointment, precisely weighing, placing the ointment into a conical flask with a plug, adding 50ml of ethanol, carrying out ultrasonic treatment (power 250W and frequency 20kHz) for 20 minutes, evaporating in a water bath until the volume is small, adding 2.5g of diatomite, uniformly stirring, drying by distillation, adding 50ml of petroleum ether (60-90 ℃) and carrying out ultrasonic treatment (power 250W and frequency 20kHz) for 20 minutes, cooling, pouring off supernate, drying residues in a water bath at 80 ℃, precisely adding 50ml of methanol, weighing the weight, carrying out ultrasonic treatment (power 250W and frequency 20kHz) for 20 minutes, cooling, weighing the weight, complementing the weight loss by methanol, shaking uniformly, filtering, and taking a subsequent filtrate and filtering by using a microporous filter membrane (0.45 mu m) to obtain the sophora japonica-scutellaria ointment.
The determination method comprises precisely sucking 20 μ l of each of the reference solution and the sample solution, injecting into liquid chromatograph, and determining.
The ointment contains fructus Sophorae (parched) and rutin (C) per lg27H30O16) Calculated, the content of the active ingredient should not be less than 1.1 mg.
The above measurement method has the following problems:
① since the Sophora japonica Linn ointment is an ointment, it contains more oil and fat components, and the extraction effect is affected by direct extraction with methanol, and the extractive solution contains a large amount of fat-soluble matrix, which pollutes the chromatographic system.
② the solubility of rutin in pure methanol is superior to other extraction solvents, and if the extraction is carried out by heating, more fat-soluble matrix is brought to the sample solution, which can seriously pollute the chromatographic system.
③ method for preparing the test solution from the original standard comprises collecting flos Sophorae radix Scutellariae ointment 1g, precisely weighing, placing in a conical flask with a plug, adding 50ml ethanol, treating with ultrasound (power 250W, frequency 20KHZ) for 20 min, evaporating in water bath to small volume, adding diatomite 2.5g, stirring, evaporating, adding 50ml petroleum ether (60-90 deg.C), treating with ultrasound (power 250W, frequency 20KHZ) for 20 min, cooling, removing supernatant, evaporating the residue in water bath at 80 deg.C, precisely adding 50ml methanol, weighing, treating with ultrasound for 20 min, cooling, weighing again, adding methanol to reduce weight, shaking, filtering, and filtering with microporous membrane (0.45 μm).
④ chromatographic conditions of pure tetrahydrofuran in the mobile phase are not commonly used in the laboratory and are more damaging to chromatographic systems.
Disclosure of Invention
In order to solve the technical problems, the invention provides a method for measuring the content of rutin in sophora baical ointment.
The invention relates to a method for measuring the content of rutin in sophora japonica-scutellaria ointment, which solves the technical problems through the following technical scheme.
The method for measuring the content of rutin in the sophora flower-scutellaria ointment comprises the following chromatographic conditions: octadecylsilane chemically bonded silica is used as a filling agent; methanol-ethanol-0.5% phosphoric acid solution (13:13:74) as mobile phase; the flow rate was 1.0mL/min, the column temperature was 30 ℃ and the detection wavelength was 359 nm. The volume ratio of the methanol-ethanol-0.5% phosphoric acid solution is 13:13: 74.
In the method for measuring the content of the rutin,
preparing test solution by weighing 3g of flos Sophorae Immaturus radix Scutellariae ointment, precisely weighing, adding 2 times of diatomaceous earth, precisely weighing, grinding, weighing 1g, precisely weighing, placing in a conical flask with a plug, precisely adding 25ml of methanol, weighing, ultrasonically treating for 30 min, cooling, weighing again, adding methanol to reduce weight, shaking, filtering, and filtering with microporous membrane to obtain the final product. In the method for measuring the content of rutin in the sophora japonica-scutellaria ointment, the ultrasonic power of ultrasonic treatment is 250W, and the frequency is 20 kHz. The aperture of the microporous filter membrane is 0.45 mu m.
The method for measuring the content of rutin in the sophora and scutellaria 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 30 ℃ and the detection wavelength was 359 nm. The number of theoretical plates is not less than 2500 calculated according to rutin peak;
preparing a reference substance solution by precisely weighing an appropriate amount of rutin reference substance, and adding methanol to obtain a solution containing 40 μ g per 1 ml;
preparing a test solution by taking 3g of sophora japonica-scutellaria ointment, precisely weighing, adding 2 times of diatomite, precisely weighing, grinding, taking about 1g of sophora japonica-scutellaria ointment, precisely weighing, placing in a conical flask with a plug, precisely adding 25ml of methanol, weighing, carrying out ultrasonic treatment (power 250W, frequency 20kHz) for 30 minutes, cooling, weighing again, supplementing the weight loss by using methanol, shaking up, filtering, and filtering a subsequent filtrate by using a microporous filter membrane (0.45 mu m) to obtain the sophora japonica-scutellaria ointment;
the determination method comprises precisely sucking 10 μ l of each of the reference solution and the sample solution, injecting into liquid chromatograph, and determining.
The 0.5 percent phosphoric acid solution is 0.5 percent phosphoric acid solution in percentage by mass.
The beneficial effect of the invention is that,
① the test solution is prepared by adsorbing oil components with diatomaceous earth, and extracting with methanol, and has good extraction effect, and avoids the influence of oil components in flos Sophorae radix Scutellariae ointment on rutin extraction, and avoids the contamination of chromatographic system due to large amount of fat-soluble matrix in the extractive solution.
② the solubility of rutin in pure methanol is superior to other extraction solvents, and if the extraction is carried out by heating, more liposoluble matrix is brought to the sample solution, which can seriously pollute the chromatographic system, so the extraction method omits the step of water bath evaporation, and avoids the harm of the more liposoluble matrix brought by the sample solution caused by heating, which can seriously pollute the chromatographic system.
③ A simplified preparation method of test solution comprises weighing 1g of Sophora japonica ointment, precisely weighing, placing in a conical flask with a plug, adding 50ml of ethanol, treating with ultrasound (power 250W, frequency 20KHZ) for 20 min, evaporating in water bath to small volume, adding 2.5g of diatomaceous earth, stirring, evaporating to dryness, adding 50ml of petroleum ether (60-90 deg.C), treating with ultrasound (power 250W, frequency 20KHZ) for 20 min, cooling, removing supernatant, evaporating the residue in water bath at 80 deg.C, precisely adding 50ml of methanol, weighing, treating with ultrasound for 20 min, cooling, weighing again, adding methanol to reduce weight loss, shaking, filtering, collecting filtrate, filtering with microporous membrane (0.45 μm), and collecting the filtrate, grinding, and directly adding methanol for ultrasonic extraction.
④ chromatographic pure tetrahydrofuran in the mobile phase in the original standard chromatographic condition is not commonly used in a laboratory and has larger damage to a chromatographic system, the original standard 'tetrahydrofuran-water-glacial acetic acid (22:78:2) is used as the mobile phase' is revised to 'methanol-acetonitrile-0.5% phosphoric acid solution (13:13:74) is used as the mobile phase', the inspection cost is reduced, and the damage to the chromatographic system is reduced.
⑤ it is ensured that the peak of rutin chromatogram in the test solution has high separation degree from other impurity peaks, and the theoretical plate number is not less than 1000 calculated according to rutin peak in the original standard is revised to be not less than 2500 calculated according to rutin peak.
⑥ ensuring that the rutin chromatographic peak area of the reference substance solution and the rutin chromatographic peak area of the test solution have a better proportional relationship, precisely weighing a proper amount of rutin reference substance which is prepared by drying the reference substance solution at 120 ℃ under reduced pressure to constant weight in the original standard, adding methanol to prepare a solution containing 20 mug per 1ml, shaking up, and modifying to obtain the rutin reference substance which is prepared by precisely weighing the proper amount of rutin reference substance and adding methanol to prepare a solution containing 40 mug per 1 ml.
Drawings
FIG. 1 is a determination test map of a mobile phase for measuring rutin content.
FIG. 2-A is a test chart of rutin content determination, a reference solution.
FIG. 2-B is a test chart of rutin content determination specificity-test solution.
FIG. 2-C is a rutin content determination specificity test pattern-negative solution.
Detailed Description
The invention will be further described with reference to the accompanying drawings and specific embodiments so that those skilled in the art may better understand the invention, but the invention is not limited thereto.
A method for measuring the content of rutin in sophora and scutellaria 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 30 ℃ and the detection wavelength was 359 nm. The number of theoretical plates is not less than 2500 calculated according to rutin peak;
preparing a reference substance solution by precisely weighing an appropriate amount of rutin reference substance, and adding methanol to obtain a solution containing 40 μ g per 1 ml;
preparing a test solution, namely taking about 3g of sophora japonica-scutellaria ointment, precisely weighing, adding about 2 times of diatomite, precisely weighing, grinding, taking about 1g of sophora japonica-scutellaria ointment, precisely weighing, placing in a conical flask with a plug, precisely adding 25ml of methanol, weighing, ultrasonically treating (the power is 250W, the frequency is 20kHz) for 30 minutes, cooling, weighing again, supplementing the weight loss by using the methanol, shaking up, filtering, taking a subsequent filtrate, and filtering by using a microporous filter membrane (0.45 mu m) to obtain the sophora japonica-scutellaria ointment;
the determination method comprises precisely sucking 10 μ l of each of the reference solution and the sample solution, injecting into liquid chromatograph, and determining. HPLC content determination methodological verification of rutin (sample batch for methodological research: 19010105)
Sophora japonica and scutellaria baicalensis ointment test solution and reference solution are prepared, and the test is carried out according to the conditions of high performance liquid chromatography 0512 in the four ministry of communications in 2015 pharmacopoeia.
1. Verifying items
a. Selecting a mobile phase; b. testing the durability of the chromatographic column; c. investigating ultrasonic time; d. examining the sampling quantity; e. investigating a linear relation; f. performing precision test; g. inspecting repeatability; h. testing the stability of the sample; i. sample adding recovery rate test; j specificity test; k sample determination
2. And (3) verification and implementation:
2.1 instruments and reagents
2.1.1 Instrument: LC-20AT HPLC; an electronic balance.
2.1.2 reagents:
methanol and acetonitrile are chromatographically pure, and other reagents are analytically pure.
2.1.3 rutin control information:
batch number: 100080-201811 with a content of 91.7%
The source is as follows: provided by the institute of food and drug testing in China.
2.2 chromatographic conditions and system applicability test using octadecylsilane chemically bonded silica as filler, 359nm detection wavelength, methanol-acetonitrile-0.5% phosphoric acid solution (13:13:74) as mobile phase, 1.0ml/min flow rate, 30 deg.C column temperature; the theoretical plate number is not lower than 2500 calculated according to rutin peak.
2.2.1 screening of the Mobile phase
Purpose determination A commonly used mobile phase methanol-acetonitrile-0.5% phosphoric acid solution (13:13:74)
2.2.1.1 preparation of control solution rutin controls ① 4.185.185 mg and ② 4.294mg are weighed precisely, put into 100ml measuring bottles respectively, dissolved and diluted to scale by adding methanol, and shaken well to obtain (C)To 1：38.37645μg/ml、CTo 2：39.37598μg/ml)。
2.2.1.2 preparation of test solution 19010105 Sophora japonica-Scutellaria ointment 3.0720g is precisely weighed, 6.0043g of diatomaceous earth is added, precisely weighed, ground, precisely weighed, ① 1.0132g and ② 0.9898g of test sample are placed in a conical flask with a plug, 25ml of methanol is precisely added, the weight is weighed, ultrasonic treatment (power 250W and frequency 20kHz) is carried out for 30 minutes, the mixture is cooled, the weight is weighed again, the weight loss is compensated by the methanol, the mixture is shaken evenly and filtered, and a subsequent filtrate is taken and filtered by a microfiltration membrane (0.45 mu m) to obtain the test solution.
2.2.1.3, precisely sucking 10 μ l of each of the reference solution and the sample solution, and injecting into a liquid chromatograph.
2.2.1.4 conclusion: the separation effect of the rutin chromatographic peak and other chromatographic peaks in the chromatogram of the test solution is better. Therefore, the mobile phase was determined to be methanol-acetonitrile-0.5% phosphoric acid solution (13:13: 74). The results are shown in FIG. 1. FIG. 1: and determining a test pattern of the mobile phase.
2.3 chromatographic column durability test
The purpose is to investigate the separation degree of rutin chromatographic peak and other impurity peak in different chromatographic column sample solutions.
2.3.1 preparation of control solutions:
2.3.1.1Thermo5 μm, 250 × 4.6.6 4.6mmC18 chromatographic column, which is prepared by collecting 2.2.1.1 items of control solution;
2.3.1.2Welch5 μm, 250 × 4.6.6 4.6mmC18 chromatographic column, precisely weighing rutin control substances ① 4.340mg and ② 4.199mg, respectively placing into 100ml measuring flask, adding methanol to dissolve and dilute to scale, and shaking uniformly to obtain (C)To 1：39.7978μg/ml、CTo 2：38.50483μg/ml)；
2.3.1.3Agela5 μm, 250 × 4.6.6 4.6mmC18 chromatographic column, precisely weighing rutin control substances ① 4.028.028 mg and ② 4.161.161 mg, respectively placing into 100ml measuring flask, dissolving in methanol, diluting to scale, and shaking to obtain the final product (C)To 1：36.93676μg/ml、CTo 2：38.15637μg/ml)。
2.3.2 preparation of test solutions:
2.3.2.1Thermo5 μm, 250 × 4.6.6 4.6mmC18 chromatographic column, which is prepared by collecting 2.2.1.2 items of test solution;
2.3.2.2Welch5 μm, 250 × 4.6.6 4.6mmC18 chromatographic column, namely, 19010105 g of sophora japonica-scutellaria ointment 3.0384g is precisely weighed, 6.0072g of diatomite is added, the precision is precisely weighed, the materials are finely ground, ① 1.0255g and ② 0.9677g of samples are precisely weighed, the samples are placed in a conical flask with a plug, 25ml of methanol is precisely added, the weight is weighed, ultrasonic treatment (the power is 250W, the frequency is 20kHz) is carried out for 30 minutes, the mixture is cooled, the weight is weighed again, the weight loss is compensated by the methanol, the mixture is shaken up and filtered, and the subsequent filtrate is taken and filtered by a microporous filter membrane (0.45 μm), thus obtaining the product;
2.3.2.3Agela5 μm, 250 × 4.6.6 4.6mmC18 chromatographic column is prepared by collecting 19010105 g of Sophora japonica ointment 3.0528g, precisely weighing, adding 6.0176g of diatomaceous earth, precisely weighing, grinding, precisely weighing ① 1.0382g and ② 1.0347.0347 g of test sample, placing in a conical flask with a plug, precisely adding 25ml of methanol, weighing, ultrasonic treating (power 250W, frequency 20kHz) for 30 min, cooling, weighing again, supplementing lost weight with methanol, shaking, filtering, and filtering with microporous membrane (0.45 μm).
2.3.3 measurement, wherein 10 μ l of the above solution is precisely pipetted and injected into a liquid chromatograph, and the solution is tested according to the above chromatographic conditions by using Thermo5 μm, 250 × 4.6.6 4.6mmC18 chromatographic column, Welch5 μm, 250 × 4.6.6 4.6mmC18 chromatographic column and Agela5 μm, 250 × 4.6.6 4.6mmC18 chromatographic column;
2.3.4 conclusion: the peak shape and the separation effect are ideal, and the theoretical plate number of the three chromatographic columns is respectively 14449, 15048 and 14547 which are not less than 2500 calculated according to rutin.
2.4 ultrasonic temporal investigation
Aims to investigate the influence of ultrasonic time on the rutin content determination result.
2.4.1 preparation of control solution rutin controls ① 4.253mg and ② 4.014.014 mg were weighed precisely, placed in 100ml measuring bottles respectively, dissolved in methanol and diluted to the scale, shaken well to obtain (C)To 1：39.00001μg/ml、CTo 2：36.80838μg/ml)。
2.4.2 preparation of test solution 19010105 Sophora japonica ointment 2.9403g was weighed precisely, 6.0154g of diatomaceous earth was added, weighed precisely, ground, and weighed precisely, test specimen ① 1.0207.0207 g, ② 1.0214g, ③ 1.0229g, ④ 1.0332g, ⑤ 1.0515g, and ⑥ 1.0425.0425 g were weighed precisely, placed in a conical flask with a stopper, 25ml of methanol was added precisely, the weight was weighed, ultrasonic treatment (power 250W, frequency 20kHz) was carried out for 20 minutes, 30 minutes, and 60 minutes, and the flask was cooled down, weighed again, the weight loss was made up with methanol, shaken well, filtered, and the subsequent filtrate was filtered with a microfiltration membrane (0.45 μm).
2.4.3 determination: precisely sucking 10 μ l of each of the above solutions, measuring under a predetermined chromatographic condition,
2.4.4 results are shown in Table 1.
TABLE 1 ultrasonic time examination of rutin content
2.4.5 conclusion: as can be seen from the above measurement results, the ultrasonic time has no difference to the measurement results, and the ultrasonic time is set for 30 minutes in order to ensure the accuracy of the measurement results by integrating various test factors.
2.5 examination of sample size
The purpose is to investigate the influence of the sample quantity on the rutin content determination result.
2.5.1 preparation of control solution rutin controls ① 4.266.266 mg, ② 4.073mg are weighed precisely, put into 100ml measuring flask respectively, dissolved and diluted to scale by adding methanol, and shaken well to obtain (C)To 1：39.11922μg/ml、CTo 2：37.34941μg/ml)。
2.5.2 preparation of test solution ① 0.5258g, ② 0.5231g, ③ 1.0388g, ④ 1.0374g, ⑤ 2.0158g and ⑥ 2.0150g of the test sample to be tested under 2.4.2 are precisely weighed and respectively placed in a conical flask with a plug, 25ml of methanol is precisely added, the weight is weighed, ultrasonic treatment (power 250W, frequency 20kHz) is carried out for 30 minutes, the mixture is cooled, the weight is weighed again, the loss weight is compensated by the methanol, the mixture is shaken up and filtered, and a subsequent filtrate is taken and filtered by a microporous filter membrane (0.45 mu m), so that the test sample is obtained.
2.5.3 determination: each 10. mu.l of the solution was precisely pipetted and measured under the specified chromatographic conditions, and the results are shown in Table 2.
TABLE 2 rutin content sample volume investigation results
2.5.4 conclusion: as can be seen from the above measurement results, there was almost no difference in the measurement results of the three kinds of sample amounts, and the sample amount was determined to be 1.0g in consideration of the error of the sample amount and the contamination of the chromatographic column.
2.6 precision test
Aims to investigate the degree of the same uniform reference substance solution among the results of multiple sampling measurement under the specified test conditions, and the RSD is less than or equal to 2.0 percent
2.6.1 preparation of control solution rutin control 4.135mg is precisely weighed, put into a 100ml measuring flask, dissolved in methanol and diluted to scale, and shaken up to obtain (C)To pair：37.91795μg/ml)。
2.6.2 determination: precisely sucking 10 μ l of control solution under item 2.6.1, injecting into liquid chromatograph, continuously sampling for 6 times, and measuring its peak area. As a result: see table 4.
TABLE 4 precision test results of rutin content
2.6.3 conclusion: the test result shows that the precision of the instrument is good.
2.7 the investigation purpose of the linear relation determines whether the concentration of the sample solution and the quantitative information are in the linear relation; determination of the linear range, i.e. the appropriate sample size. 2.7.1 determination: the control solutions 1, 2, 5, 10, 15 and 20. mu.l under 2.6.1 were precisely pipetted and injected into a liquid chromatograph, and the peak areas were measured.
2.7.2 taking the sample amount of rutin control as abscissa and peak area integral value as ordinate, and performing linear regression to obtain rutin regression equation y of 2 × 106x-2516.2, correlation coefficient R2See table 3 for 1.
TABLE 3 rutin Linear relationship examination results
2.7.3 conclusion: the rutin sample amount is 0.037918-0.758359 mu g, and the peak area integral value is in a good linear relation.
2.8 repeatability test
Aiming at investigating the precision of the detection result of an experimenter under the same condition
2.8.1 preparation of control solution rutin controls ① 4.003mg, ② 4.041mg are weighed precisely, put into 100ml measuring flask respectively, dissolved and diluted to scale by adding methanol, and shaken well to obtain (C)To 1：36.70751μg/ml、CTo 2：37.05597μg/ml)。
2.8.2 preparation of test solution ① 1.0135g, ② 1.0133g, ③ 1.0261g, ④ 1.0234g, ⑤ 1.0200g and ⑥ 1.0359g of the test sample to be tested under 2.4.2 are precisely weighed, placed in a conical flask with a plug, 25ml of methanol is precisely added respectively, the weight is weighed, ultrasonic treatment (power 250W, frequency 20kHz) is carried out for 30 minutes, the mixture is cooled, the weight is weighed again, the loss weight is compensated by the methanol, the mixture is shaken up and filtered, and the subsequent filtrate is filtered by a microporous filter membrane (0.45 mu m), thus obtaining the test solution.
2.8.3 measuring, precisely sucking 10 μ l of reference substance and sample solution, respectively, injecting into liquid chromatograph, measuring, and calculating content. The results are shown in Table 5.
TABLE 5 repeatability test results for rutin content
2.8.4 conclusion: as can be seen from the above measurement results, the method was excellent in reproducibility.
2.9 sample stability test
The stability of the component to be detected in the detection process of the sample solution is inspected.
2.9.1 the test solution 1 under the item of the repeatability test 2.8.2 is taken as the test solution.
2.9.2 determination: injecting sample once every a period of time, 10 mul each time, measuring the peak area of rutin, and totally inspecting for 24 hours. The results are shown in Table 6.
Table 6 stability test results of rutin content
2.9.3 conclusion: the test result shows that the test solution has good stability within 24 hours and can meet the requirement of rutin content determination.
2.10 sample recovery test
The aim is to investigate whether the sample recovery rate meets the requirements.
2.10.1 preparation of control solution rutin controls ① 4.050.050 mg and ② 4.117.117 mg are weighed precisely, placed in 100ml measuring bottles respectively, dissolved in methanol and diluted to scale, and shaken well to obtain (C)To 1：37.1385μg/ml、CTo 2：37.75289μg/ml)。
2.10.2 preparation of control stock solution rutin control 6.031mg is precisely weighed, put into a 250ml measuring flask, dissolved in methanol and diluted to scale, and shaken up to obtain (C)To pair：0.022122mg/ml)。
2.10.3 preparation of test solution 19010105 flos Sophorae Immaturus and Scutellariae radix ointment 2.9728g (with known rutin content of 3.6mg/g), adding diatomaceous earth 6.0045g, grinding, precisely weighing ① 0.4689g, ② 0.4655g, ③ 0.4828g, ④ 0.4912g, ⑤ 0.4841g and ⑥ 0.5131g, placing in a conical flask with a plug, precisely adding control stock solution 25ml, weighing, ultrasonic treating (power 250W and frequency 20kHz) for 30 min, cooling, weighing again, supplementing lost weight with methanol, shaking, filtering, and filtering with microporous membrane (0.45 μm).
2.10.4 the test solution was precisely extracted 10. mu.l each of the control and test solutions, and the solution was injected into a liquid chromatograph, and the measurement was carried out by the above-mentioned method to calculate the recovery rate. The results are shown in Table 7.
TABLE 7 rutin loading recovery test results
2.10.5 conclusion: the test result shows that the sample recovery rate test of the determination method is good.
2.11 specificity test
Aim to investigate whether the auxiliary materials interfere with the determination result
2.11.1 preparation of control solution rutin controls ① 4.096.096 mg and ② 4.296mg are weighed precisely, put into 100ml measuring bottles respectively, dissolved in methanol and diluted to scale, and shaken well to obtain (C)To 1：37.56032μg/ml、CTo 2：39.39432μg/ml)。
2.11.2 preparation of test solution 19010105 Sophora japonica-Scutellariae ointment 3.0295g was weighed precisely, 6.0014g of diatomaceous earth was added, weighed precisely, ground, and weighed precisely, test sample 1.0400g was weighed precisely, placed in a conical flask with a stopper, methanol 25ml was added precisely, weighed, sonicated (power 250W, frequency 20kHz) for 30 minutes, allowed to cool, weighed again, the loss of weight was made up with methanol, shaken well, filtered, and the subsequent filtrate was filtered through a microfiltration membrane (0.45 μm).
2.11.3 preparation of negative control solution the other medicines except fructus Sophorae (parched) in the prescription are removed, 3.1189g negative sample without fructus Sophorae (parched) is prepared according to the prescription proportion, 6.0014g diatomite is added, ground and precisely weighed 1.0055g, and the negative control solution is prepared by the same method as the preparation of the test solution.
2.11.4 the measurement was carried out by precisely sucking 10. mu.l of each of the above-mentioned control solution, test solution and negative control solution, and injecting the solution into a liquid chromatograph for measurement.
2.11.5 results: the chromatogram of the test sample has a corresponding chromatographic peak at the same position as the retention time of the chromatogram of the control sample, and the chromatogram of the negative control has no corresponding chromatographic peak of the control. The map is shown in FIG. 2.
2.11.6 conclusion: the other medicinal ingredients in the prescription have no interference to the measurement result.
2.12 sample determination
2.12.1 batch number: 18100105, respectively; 190101051, respectively; 190401051 HUAQIN ointment
2.12.2.1 preparation of control solution rutin controls ① 4.025.025 mg and ② 4.107mg are weighed precisely, put into 100ml measuring bottles respectively, dissolved and diluted to scale by adding methanol, and shaken well to obtain (C)To 1：36.90925μg/ml、CTo 2：37.66119μg/ml)。
2.12.2.2 preparation of test solution
2.12.2.2.1 weighing 18100105 flos Sophorae Immaturus ointment 3.0839g precisely, weighing precisely, adding 6.0678g diatomaceous earth, weighing precisely, grinding, weighing ① 0.9985.9985 g test sample and ② 0.9994.9994 g precisely, placing in a conical flask with a plug, adding methanol 25ml precisely, weighing, ultrasonic treating (power 250W, frequency 20kHz) for 30 min, cooling, weighing again, adding methanol to compensate the weight loss, shaking, filtering, and filtering with microporous membrane (0.45 μm).
2.12.2.2.2 precisely weighing 190101051 HUAIQI ointment 3.0295g, precisely weighing, adding 6.0014g diatomaceous earth, precisely weighing, grinding, precisely weighing test sample ① 0.9388g and ② 0.9339g, placing in a conical flask with a plug, precisely adding 25ml methanol, weighing, ultrasonic treating (power 250W, frequency 20kHz) for 30 min, cooling, weighing, supplementing the weight loss with methanol, shaking, filtering, and filtering with microporous membrane (0.45 μm).
2.12.2.2.3 precisely weighing 190401051 flos Sophorae Immaturus ointment 3.1011g, precisely weighing, adding 6.0231g diatomaceous earth, precisely weighing, grinding, precisely weighing test sample ① 0.9989.9989 g and ② 0.9783g, placing in a conical flask with a plug, precisely adding 25ml methanol, weighing, ultrasonic treating (power 250W, frequency 20kHz) for 30 min, cooling, weighing again, adding methanol to reduce weight, shaking, filtering, and filtering with microporous membrane (0.45 μm).
2.12.2.3 the measurement was carried out by precisely sucking 10. mu.l of each of the above-mentioned control solution, test solution and negative control solution, and injecting the solution into a liquid chromatograph for measurement.
2.12.3 results: see table 8.
TABLE 8 rutin content measurement results of three samples
2.12.4 conclusion: the national standard stipulates that every 1g of the medicine contains rutin (C) in the form of fructus Sophorae (parched)27H30O16) And in the method, the content of the sample is not less than 1.1mg, and the content of 3 batches of samples is measured to be within the range of 3.1-4.1 mg/g according to the revised preparation method of the sample solution.
Claims (7)
1. A method for measuring the content of rutin in sophora and scutellaria ointment is characterized in that the method for measuring the content of rutin is a high performance liquid chromatography.
2. The method for measuring the content of rutin in the sophora japonica-scutellaria ointment according to claim 1, wherein the chromatographic conditions of the method for measuring the content of rutin are as follows: octadecylsilane chemically bonded silica is used as a filling agent; methanol-ethanol-0.5% phosphoric acid solution (13:13:74) as mobile phase; the flow rate was 1.0mL/min, the column temperature was 30 ℃ and the detection wavelength was 359 nm.
3. The method for determining the content of rutin in the sophora japonica-scutellaria ointment according to claim 1, wherein the volume ratio of the methanol-ethanol-0.5% phosphoric acid solution is 13:13: 74.
4. The method for measuring the content of rutin in the sophora japonica-scutellaria ointment according to claim 1, wherein in the method for measuring the content of rutin, a preparation method of a test solution comprises the following steps: precisely weighing 3g of sophora japonica-scutellaria ointment, adding 2 times of diatomite, precisely weighing, grinding, precisely weighing 1g of sophora japonica-scutellaria ointment, placing the sophora japonica-scutellaria ointment into a conical flask with a plug, precisely adding 25ml of methanol, weighing, ultrasonically treating for 30 minutes, cooling, weighing again, supplementing the weight loss by using methanol, shaking up, filtering, and filtering the subsequent filtrate by using a microporous filter membrane to obtain the sophora japonica-scutellaria ointment.
5. The method for determining the content of rutin in the sophora japonica-scutellaria ointment according to claim 4, wherein the ultrasonic power of the ultrasonic treatment is 250W, and the frequency is 20 kHz.
6. The method for determining the content of rutin in the sophora japonica-scutellaria ointment according to claim 4, wherein the pore size of the microporous filter membrane is 0.45 μm.
7. The method for measuring the content of rutin in the sophora japonica-scutellaria ointment according to claim 1, wherein the method 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 is 1.0mL/min, the column temperature is 30 ℃, and the detection wavelength is 359 nm; the number of theoretical plates is not less than 2500 calculated according to rutin peak;
preparing a reference solution by adding methanol into a rutin reference to prepare a solution containing 40 mug of rutin per 1 ml;
preparing a test solution by taking 3g of sophora japonica-scutellaria ointment, precisely weighing, adding 2 times of diatomite, precisely weighing, grinding, taking about 1g of sophora japonica-scutellaria ointment, precisely weighing, placing in a conical flask with a plug, precisely adding 25ml of methanol, weighing, carrying out ultrasonic treatment (power 250W, frequency 20kHz) for 30 minutes, cooling, weighing again, supplementing the weight loss by using methanol, shaking up, filtering, and filtering a subsequent filtrate by using a microporous filter membrane (0.45 mu m) to obtain the sophora japonica-scutellaria ointment;
the determination method comprises precisely sucking 10 μ l of each of the reference solution and the sample solution, injecting into liquid chromatograph, and determining.
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