CN115541745B - Quality detection method for hypericum perforatum standard decoction and formula particles - Google Patents
Quality detection method for hypericum perforatum standard decoction and formula particles Download PDFInfo
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- CN115541745B CN115541745B CN202211143803.3A CN202211143803A CN115541745B CN 115541745 B CN115541745 B CN 115541745B CN 202211143803 A CN202211143803 A CN 202211143803A CN 115541745 B CN115541745 B CN 115541745B
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- hypericum perforatum
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- hyperforin
- quality
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- 239000002245 particle Substances 0.000 title claims abstract description 34
- 238000001514 detection method Methods 0.000 title claims abstract description 17
- 235000017309 Hypericum perforatum Nutrition 0.000 title claims description 43
- 244000141009 Hypericum perforatum Species 0.000 title claims description 42
- 239000013558 reference substance Substances 0.000 claims abstract description 37
- 239000012488 sample solution Substances 0.000 claims abstract description 30
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- 238000001228 spectrum Methods 0.000 claims abstract description 20
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- 240000007673 Origanum vulgare Species 0.000 claims abstract description 8
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- 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 claims abstract description 8
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- 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 claims abstract description 8
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 42
- 239000000243 solution Substances 0.000 claims description 28
- PZIRUHCJZBGLDY-UHFFFAOYSA-N Caffeoylquinic acid Natural products CC(CCC(=O)C(C)C1C(=O)CC2C3CC(O)C4CC(O)CCC4(C)C3CCC12C)C(=O)O PZIRUHCJZBGLDY-UHFFFAOYSA-N 0.000 claims description 26
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- CWVRJTMFETXNAD-JUHZACGLSA-N chlorogenic acid Chemical compound O[C@@H]1[C@H](O)C[C@@](O)(C(O)=O)C[C@H]1OC(=O)\C=C\C1=CC=C(O)C(O)=C1 CWVRJTMFETXNAD-JUHZACGLSA-N 0.000 claims description 20
- 229940074393 chlorogenic acid Drugs 0.000 claims description 20
- FFQSDFBBSXGVKF-KHSQJDLVSA-N chlorogenic acid Natural products O[C@@H]1C[C@](O)(C[C@@H](CC(=O)C=Cc2ccc(O)c(O)c2)[C@@H]1O)C(=O)O FFQSDFBBSXGVKF-KHSQJDLVSA-N 0.000 claims description 20
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- 238000005303 weighing Methods 0.000 claims description 19
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- YQUVCSBJEUQKSH-UHFFFAOYSA-N 3,4-dihydroxybenzoic acid Chemical compound OC(=O)C1=CC=C(O)C(O)=C1 YQUVCSBJEUQKSH-UHFFFAOYSA-N 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- OVSQVDMCBVZWGM-SJWGPRHPSA-N Hyperin Natural products O[C@H]1[C@H](O)[C@@H](O)[C@@H](CO)O[C@H]1OC1=C(C=2C=C(O)C(O)=CC=2)OC2=CC(O)=CC(O)=C2C1=O OVSQVDMCBVZWGM-SJWGPRHPSA-N 0.000 claims description 15
- OVSQVDMCBVZWGM-DTGCRPNFSA-N quercetin 3-O-beta-D-galactopyranoside Chemical compound O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@H]1OC1=C(C=2C=C(O)C(O)=CC=2)OC2=CC(O)=CC(O)=C2C1=O OVSQVDMCBVZWGM-DTGCRPNFSA-N 0.000 claims description 15
- BBFYUPYFXSSMNV-UHFFFAOYSA-N quercetin-7-o-galactoside Natural products OC1C(O)C(O)C(CO)OC1OC1=CC(O)=C2C(=O)C(O)=C(C=3C=C(O)C(O)=CC=3)OC2=C1 BBFYUPYFXSSMNV-UHFFFAOYSA-N 0.000 claims description 15
- REFJWTPEDVJJIY-UHFFFAOYSA-N Quercetin Chemical compound C=1C(O)=CC(O)=C(C(C=2O)=O)C=1OC=2C1=CC=C(O)C(O)=C1 REFJWTPEDVJJIY-UHFFFAOYSA-N 0.000 claims description 14
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- 238000009210 therapy by ultrasound Methods 0.000 claims description 9
- GYFFKZTYYAFCTR-JUHZACGLSA-N 4-O-trans-caffeoylquinic acid Chemical compound O[C@@H]1C[C@](O)(C(O)=O)C[C@@H](O)[C@H]1OC(=O)\C=C\C1=CC=C(O)C(O)=C1 GYFFKZTYYAFCTR-JUHZACGLSA-N 0.000 claims description 8
- GYFFKZTYYAFCTR-UHFFFAOYSA-N 5-O-(6'-O-galloyl)-beta-D-glucopyranosylgentisic acid Natural products OC1CC(O)(C(O)=O)CC(O)C1OC(=O)C=CC1=CC=C(O)C(O)=C1 GYFFKZTYYAFCTR-UHFFFAOYSA-N 0.000 claims description 8
- OVSQVDMCBVZWGM-IDRAQACASA-N Hirsutrin Natural products O([C@H]1[C@H](O)[C@H](O)[C@H](O)[C@@H](CO)O1)C1=C(c2cc(O)c(O)cc2)Oc2c(c(O)cc(O)c2)C1=O OVSQVDMCBVZWGM-IDRAQACASA-N 0.000 claims description 8
- GYFFKZTYYAFCTR-LMRQPLJMSA-N cryptochlorogenic acid Natural products O[C@H]1C[C@@](O)(C[C@H](O)[C@H]1OC(=O)C=Cc2ccc(O)c(O)c2)C(=O)O GYFFKZTYYAFCTR-LMRQPLJMSA-N 0.000 claims description 8
- GXMWXESSGGEWEM-UHFFFAOYSA-N isoquercitrin Natural products OCC(O)C1OC(OC2C(Oc3cc(O)cc(O)c3C2=O)c4ccc(O)c(O)c4)C(O)C1O GXMWXESSGGEWEM-UHFFFAOYSA-N 0.000 claims description 8
- OVSQVDMCBVZWGM-QSOFNFLRSA-N quercetin 3-O-beta-D-glucopyranoside Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC1=C(C=2C=C(O)C(O)=CC=2)OC2=CC(O)=CC(O)=C2C1=O OVSQVDMCBVZWGM-QSOFNFLRSA-N 0.000 claims description 8
- ZVOLCUVKHLEPEV-UHFFFAOYSA-N Quercetagetin Natural products C1=C(O)C(O)=CC=C1C1=C(O)C(=O)C2=C(O)C(O)=C(O)C=C2O1 ZVOLCUVKHLEPEV-UHFFFAOYSA-N 0.000 claims description 7
- HWTZYBCRDDUBJY-UHFFFAOYSA-N Rhynchosin Natural products C1=C(O)C(O)=CC=C1C1=C(O)C(=O)C2=CC(O)=C(O)C=C2O1 HWTZYBCRDDUBJY-UHFFFAOYSA-N 0.000 claims description 7
- 239000000706 filtrate Substances 0.000 claims description 7
- MWDZOUNAPSSOEL-UHFFFAOYSA-N kaempferol Natural products OC1=C(C(=O)c2cc(O)cc(O)c2O1)c3ccc(O)cc3 MWDZOUNAPSSOEL-UHFFFAOYSA-N 0.000 claims description 7
- 235000005875 quercetin Nutrition 0.000 claims description 7
- 229960001285 quercetin Drugs 0.000 claims description 7
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- GWTUHAXUUFROTF-UHFFFAOYSA-N pseudochlorogenic acid Natural products C1C(O)C(O)C(O)CC1(C(O)=O)OC(=O)C=CC1=CC=C(O)C(O)=C1 GWTUHAXUUFROTF-UHFFFAOYSA-N 0.000 claims description 6
- CWVRJTMFETXNAD-NXLLHMKUSA-N trans-5-O-caffeoyl-D-quinic acid Chemical compound O[C@H]1[C@H](O)C[C@](O)(C(O)=O)C[C@H]1OC(=O)\C=C\C1=CC=C(O)C(O)=C1 CWVRJTMFETXNAD-NXLLHMKUSA-N 0.000 claims description 6
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- NQYPTLKGQJDGTI-FCVRJVSHSA-N hyperoside Natural products OC[C@H]1O[C@@H](OC2=C(Oc3cc(O)cc(O)c3[C@H]2O)c4ccc(O)c(O)c4)[C@H](O)[C@@H](O)[C@H]1O NQYPTLKGQJDGTI-FCVRJVSHSA-N 0.000 claims description 4
- LUJAXSNNYBCFEE-UHFFFAOYSA-N Quercetin 3,7-dimethyl ether Natural products C=1C(OC)=CC(O)=C(C(C=2OC)=O)C=1OC=2C1=CC=C(O)C(O)=C1 LUJAXSNNYBCFEE-UHFFFAOYSA-N 0.000 claims description 3
- PUTDIROJWHRSJW-UHFFFAOYSA-N Quercitrin Natural products CC1OC(Oc2cc(cc(O)c2O)C3=CC(=O)c4c(O)cc(O)cc4O3)C(O)C(O)C1O PUTDIROJWHRSJW-UHFFFAOYSA-N 0.000 claims description 3
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Classifications
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- 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
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- G—PHYSICS
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- 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
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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
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Abstract
The invention discloses a quality detection method of a standard hyperforin decoction and formula particles, which comprises the steps of preparing a sample solution of hyperforin, preparing a reference substance solution of a reference substance, and obtaining a characteristic spectrum of the sample solution by adopting an ultra-high performance liquid chromatography, wherein the characteristic spectrum at least comprises 11 characteristic peaks. The invention carries out quality control on the standard hyperforin decoction and the formula particles through 11 characteristic peaks, and systematically reflects the chemical component general appearance of the hyperforin formula particles. The quality of the hyperforin recipe granule can be evaluated more accurately and objectively, the false oregano in the hyperforin recipe granule can be identified rapidly and effectively, and compared with the single rutin content index in Chinese pharmacopoeia, the quality control can be performed more efficiently, and the effectiveness of clinical medication can be ensured.
Description
Technical Field
The invention relates to a quality detection method of medicinal materials, in particular to a quality detection method of a standard hyperforin decoction and formula particles.
Background
Hypericum perforatum is the dry aerial part of Hypericum perforatum Hypericum perforatum L, belonging to Guttiferae, and also called Hypericum perforatum, hypericum parvifolia, etc., and the wiener is carried in Zhuqian dictionary. European is called san Jose grass. It is cold in nature, pungent in flavor, enters liver meridian, and has the actions of soothing liver, relieving depression, clearing heat, promoting diuresis, relieving swelling and promoting lactation. Is mainly used for treating liver qi stagnation, emotional disorder, heart-chest depression, joint swelling and pain, acute mastitis and hypogalactia.
The quality research literature of Hypericum perforatum mainly comprises: and (3) measuring the content of components such as phloroglucinol compounds (hypericin and pseudohypericin), flavonoid compounds (hyperin and rutin) and the like. Because hypericin is a phloroglucinol compound which is extremely unstable to light and heat, the content of the formula particles is extremely low, and the hypericin is not suitable for being used as a quality index. The quality of Hypericum perforatum cannot be fully characterized with flavonoid components alone.
The traditional Chinese medicine formula granule is a novel formula medicine with unified specification, unified dosage and unified quality standard, which is prepared by taking traditional Chinese medicine decoction pieces as raw materials and water as solvent through the production processes of extraction, concentration, drying, granulation and the like. The traditional Chinese medicine decoction is based on a traditional Chinese medicine standard decoction, is used under the guidance of a traditional Chinese medicine theory, and has the characteristics of convenience in taking, easiness in storage, portability, controllable quality and the like compared with the traditional Chinese medicine decoction.
At present, the quality research of the hypericum perforatum reported in the literature aims at raw medicinal materials and alcohol extracts, and research reports of quality control of water-soluble components of the hypericum perforatum are not consulted. The traditional clinical medicine mostly adopts the form of decoction, and the basis for the efficacy of the hypericum perforatum is mainly water-soluble components. Therefore, the quality control is comprehensively carried out on the water-soluble components in the hypericum perforatum, and the curative effect of clinical medication can be ensured.
The production place and the growth environment of the origanum vulgare origannm Vulagare L and the hypericum perforatum of the Labiatae are overlapped to a great extent, the appearance of the origanum vulgare origannm Vulagare L and the hypericum perforatum are similar, and the origanum vulgare origannm Vulagare L and the hypericum perforatum are stock varieties of clinical pharmacy and are easy to be confused in preparation. At present, the property identification and the physicochemical identification of the original plants and the medicinal decoction pieces are reported to be mainly carried out, the property identification depends on experienced traditional Chinese medicine identification personnel, the appearance is similar and easy to make mistakes, the property identification and the physicochemical identification can only be used for raw materials, the accuracy is low, and the property identification of the water extract and the formula particles which lose the property of the decoction pieces is difficult to identify.
Disclosure of Invention
The invention aims to: the invention aims to provide a simple, quick, efficient and accurate quality detection method for the hypericum perforatum standard decoction and formula particles, which improves the quality controllability of hypericum perforatum formula particle medicines and is beneficial to quality supervision and management.
The technical scheme is as follows: the invention relates to a quality detection method of a standard hyperforin decoction and formula particles, which comprises the following steps: preparing a sample solution of Hypericum perforatum, preparing a reference substance solution of a reference substance, and obtaining a characteristic map of the sample solution by adopting an ultra-high performance liquid chromatography; the characteristic spectrum at least comprises 11 characteristic peaks including protocatechuic acid, neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, rutin, hyperoside, isoquercitrin, quercitrin and quercetin.
Further, the retention times of the 11 characteristic peaks are respectively: the relative retention times of 5 characteristic peaks were 0.51.+ -. 10%, 0.63.+ -. 10%, 1.00, 1.12.+ -. 10% and 1.33.+ -. 10% when the characteristic peak in which chlorogenic acid was present was taken as reference peak S1, and the relative retention times of the other 6 characteristic peaks were 0.98.+ -. 10%, 1.00, 1.03.+ -. 10%, 1.18.+ -. 10%, 1.21.+ -. 10% and 1.73.+ -. 10% when the characteristic peak in which hyperin was present was taken as reference peak S2.
Further, the chromatographic conditions of the ultra-high performance liquid chromatography are as follows:
Chromatographic column: chromatographic column with octadecylsilane chemically bonded silica as filler; acetonitrile as mobile phase a and 0.01% phosphoric acid solution as mobile phase B, elution was performed according to the following gradient elution procedure:
further, the preparation method of the reference substance solution of the reference substance comprises the following steps: taking a hyperin reference substance and a chlorogenic acid reference substance, precisely weighing, and respectively adding methanol to prepare solutions containing 10-100 mug of hyperin and 5-50 mug of chlorogenic acid per 1ml of the solutions serving as reference substance solutions of the reference substances.
Further, the preparation process of the sample solution comprises the following steps: taking a test sample, adding a solvent, uniformly mixing, sealing, weighing, carrying out ultrasonic treatment, cooling, weighing again, supplementing the lost weight with the solvent, shaking uniformly, and filtering to obtain a filtrate, wherein the filtrate is the test sample solution.
Further, the mass volume ratio of the test sample to the solvent is 0.1-0.5 g: 25-100 ml.
Further, the solvent is a methanol aqueous solution with the mass concentration of 0-100% or an ethanol aqueous solution with the mass concentration of 0-100%.
Further, the power of the ultrasonic treatment is 250-300W, the frequency is 40kHz, the ultrasonic treatment time is 15-60min, and the heating reflux time is 15-60min.
Further, the sample injection volume of the reference substance solution of the reference substance is 1-5 mu L, and the sample injection volume of the sample solution of the test substance is 1-5 mu L.
The quality detection method of the standard hyperforin decoction and the formula particles can be applied to distinguishing hyperforin from pseudo-origanum.
The beneficial effects are that: compared with the prior art, the invention has the following remarkable advantages: (1) The quality detection method systematically reflects the overall appearance of chemical components of the hyperforin formulation particles, and comprises at least 11 characteristic peaks of protocatechuic acid, neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, rutin, hyperoside, isoquercitrin, quercitrin, quercetin and the like, thereby providing a basis for evaluating or controlling the quality of the hyperforin formulation particles; (2) The invention further optimizes the chromatographic conditions for obtaining the characteristic spectrum, including the optimization of mobile phase and the optimization of gradient elution program, thereby greatly shortening the analysis time, effectively improving the peak shape and the chromatographic peak separation degree, and having the characteristics of simple operation, rich spectrum information, strong characteristics and good reproducibility; (3) The method of the invention can also effectively realize the quality control in the production process, and specifically comprises the following steps: the quality control of intermediate products (extracting solution, concentrated solution and dry powder) in the preparation process of the formula particles can be effectively realized, and the components of the finally prepared hyperforin formula particles can be basically consistent with the standard decoction through the evaluation of the number of characteristic peaks and the relative peak areas, so that the curative effect consistency of the hyperforin formula particles and the traditional decoction is ensured; (4) The method can rapidly and accurately identify the hyperforin formula particles losing the property of the decoction pieces and the mixed pseudo-origanum vulgare, monitor the quality of the hyperforin formula particles and prevent feeding errors.
Drawings
FIG. 1 is a superimposed profile of a standard decoction of 15 batches of Hypericum perforatum in example 1 of the present invention;
FIG. 2 is a graph showing the characteristics of a fit control of 15 batches of Hypericum perforatum standard decoction according to example 1 of the present invention;
FIG. 3 is a characteristic spectrum of the control solution and the test solution in example 1 of the present invention;
FIG. 4 is a characteristic spectrum of 3 batches of Hypericum perforatum formula particles in example 2 of the invention;
FIG. 5 is a characteristic spectrum of a different liquid chromatograph in example 3 of the present invention;
FIG. 6 is a characteristic spectrum of a different chromatographic column in example 3 of the invention;
FIG. 7 is a graph showing the characteristics of different flow rates in example 3 of the present invention;
FIG. 8 is a characteristic spectrum of different column temperatures in example 3 of the present invention;
FIG. 9 is a graph showing the comparison of the characteristic patterns of the standard decoction of Hypericum perforatum and Oregano in example 4 of the present invention.
Detailed Description
The technical scheme of the invention is further described below with reference to the accompanying drawings.
Example 1
A quality detection method of standard decoction of herba Hyperici perforati comprises preparing sample solution of herba Hyperici perforati, preparing reference substance solution of reference substance, and obtaining characteristic spectrum of sample solution by ultra high performance liquid chromatography, wherein the characteristic spectrum at least comprises 11 characteristic peaks corresponding to protocatechuic acid, neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, rutin, hyperoside, isoquercitrin, quercetin, etc. Specifically, the chromatographic conditions of the ultra performance liquid chromatography in this embodiment are: octadecylsilane chemically bonded silica is used as filler (column length is 100mm, column inner diameter is 2.1mm, and particle diameter is 1.8 μm); eluting with ethanol as mobile phase A and 0.01% phosphoric acid as mobile phase B according to the following table 1; the flow rate is 0.25ml per minute; the column temperature is 25 ℃; the detection wavelength was 300nm.
TABLE 1
The preparation process of the reference substance solution of the reference substance comprises the following steps: taking proper amounts of hyperin reference substance and chlorogenic acid reference substance, precisely weighing, and respectively adding methanol to obtain solutions containing 40 μg and 15 μg of hyperin and chlorogenic acid per 1 ml.
The preparation process of the sample solution comprises the following steps: taking a proper amount of a standard hyperforin decoction sample, grinding, taking about 0.2g, precisely weighing, placing into a conical flask with a plug, precisely adding 25ml of 70% by mass concentration methanol water solution, sealing, weighing, performing ultrasonic treatment (power 300W, frequency 40 kHz) for 30 minutes, taking out, cooling, weighing again, supplementing the weight of the sample with 70% methanol, shaking uniformly, filtering, and taking the subsequent filtrate as a sample solution.
Precisely sucking 1 μl of reference substance solution and 1 μl of sample solution, and sampling according to the above chromatographic conditions to obtain characteristic map of 15 batches of standard decoction of herba Hyperici perforati. Adopting a traditional Chinese medicine chromatographic fingerprint similarity evaluation system (2012.1 version), taking an S1 liquid phase spectrum in 15 batches of hypericum perforatum standard decoction liquid phase spectrums as a reference spectrum, calculating according to a median to obtain a hypericum perforatum standard decoction reference spectrum, and marking common peaks, wherein 11 common peaks are marked in total, as shown in figures 1 and 2; and the retention time of each characteristic peak in the liquid phase diagram corresponding to each sample is obtained, and meanwhile, the relative retention time of each characteristic peak is calculated, as shown in table 2.
TABLE 2
As can be seen from table 2: the difference of the relative retention time of each characteristic peak is smaller and is within +/-10%, so that the quality control requirement is met. And, one batch of the sample solution and the reference solution are adopted for detection, the detection result is shown in figure 3, and by comparing each characteristic peak in the reference solution and the sample solution in figure 3, the peak 1 is protocatechuic acid, the peak 2 is neochlorogenic acid, the peak 3 is chlorogenic acid, the peak 4 is cryptochlorogenic acid, the peak 6 is rutin, the peak 7 is hyperin, the peak 8 is isoquercitrin, the peak 10 is quercetin, and the peak 11 is quercetin are respectively determined.
The preparation process of the reference substance solution comprises the following steps: and (3) taking appropriate amounts of chlorogenic acid reference substance, new chlorogenic acid reference substance, cryptochlorogenic acid reference substance, isoquercitrin reference substance and protocatechuic acid reference substance, precisely weighing, and adding methanol to prepare solutions containing 15 mug of chlorogenic acid, 10 mug of new chlorogenic acid, 15 mug of cryptochlorogenic acid, 10 mug of isoquercitrin and 15 mug of protocatechuic acid in each 1 ml.
Example 2
A quality detection method of Hypericum perforatum formula granule comprises the following steps:
(1) Preparation of test solution: taking 3 batches of hypericum perforatum prescription granules, grinding a proper amount of test sample, taking about 0.15g, precisely weighing, placing into a conical bottle with a plug, precisely adding 25ml of 70% by mass concentration methanol water solution, sealing, weighing, performing ultrasonic treatment (power 300W and frequency 40 kHz) for 30 minutes, taking out, cooling, weighing again, supplementing the lost weight with 70% by mass concentration methanol water solution, shaking uniformly, filtering, and taking the subsequent filtrate as the test sample solution.
(2) Preparation of a reference solution for a control: taking proper amounts of hyperin reference substance and chlorogenic acid reference substance, precisely weighing, and respectively adding methanol to obtain solutions containing 30 μg and 10 μg of chlorogenic acid per 1 ml.
(3) Chromatographic conditions: as in example 1.
The characteristic spectrum of 3 batches of hyperforin formula particles is obtained (figure 4), the relative retention time is calculated by taking the characteristic peaks 1,2, 4 and 5 as the S1 peak and the peak number 3 (chlorogenic acid), the relative retention time is calculated by taking the peak number 6, 8, 9, 10 and 11 as the S2 peak, and the characteristic spectrum at least comprises 11 characteristic peaks corresponding to protocatechuic acid, neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, rutin, hyperin, isoquercitrin, quercetin and the like by combining the relative retention time of the characteristic peaks (table 3) and a reference substance.
Table 33 characteristics map of Hypericum perforatum formula particle (relative retention time)
Comparing 3 batches of hypericum perforatum formula particles with the hypericum perforatum standard decoction feature patterns in the example 1, the patterns of the hypericum perforatum formula particles and the hypericum perforatum standard decoction feature patterns have good correlation, and 11 feature peaks exist in the standard decoction, which indicates that the water-soluble components in the 3 batches of hypericum perforatum formula particles are basically consistent with the standard decoction, the process is reasonable, and the formula particles can be used as substitutes of the traditional standard decoction.
Example 3
The sample solution preparation, precision, repeatability, stability and durability of the feature map are verified, and the feature map is specifically as follows:
(1) Preparation of test solution for investigation
Taking a proper amount of a test sample of hypericum perforatum prescription granule, grinding, taking about 0.15g, precisely weighing, placing into a conical bottle with a plug, precisely adding water, 30% by mass concentration of methanol aqueous solution, 50% by mass concentration of methanol aqueous solution, 70% by mass concentration of methanol aqueous solution, methanol, 30% by mass concentration of ethanol aqueous solution, 50% by mass concentration of ethanol aqueous solution, 75% by mass concentration of ethanol aqueous solution and 25ml of ethanol, sealing, weighing, performing ultrasonic treatment (power 300W, frequency 40 kHz) for 30 minutes, taking out, cooling, weighing again, supplementing the reduced weight with the corresponding solvent, shaking uniformly, filtering, taking the continuous filtrate as the test sample solution, and performing sample injection analysis. The results show that 11 characteristic peaks can be shown by using different extraction solvents, and the highest extraction efficiency of the 70% mass concentration methanol aqueous solution is obtained according to the sum of peak areas, so that the extraction solvent is preferably the 70% mass concentration methanol aqueous solution.
(2) Precision of
Taking the same sample solution in example 2, continuously sampling for 6 times to obtain a characteristic spectrum, wherein the correspondence between peak 3, peak 6, peak 7, peak 10 and peak 11 and the corresponding control solution chromatographic peaks are examined, peak 1, peak 2, peak 4 and peak 5 take peak 3 as S1 peak, peak 8 and peak 9 take peak 7 as S2 peak, calculating relative retention time and relative peak area, and calculating RSD, and the results are shown in the following tables 4 and 5.
The results show that the relative retention time and the relative peak area have RSD values of less than 3%, which indicates that the instrument method is stable and the precision is good.
TABLE 4 precision results (relative retention time)
TABLE 5 precision results (relative peak area)
(3) Repeatability of
Taking the same batch of hyperforin hypericum formula particles in example 2, precisely weighing 6 parts, preparing 6 parts of sample solutions in parallel according to the sample solution preparation method in example 1, and injecting samples respectively. Peak 1, peak 2, peak 4, peak 5 and peak 8, peak 9 and peak 7 were respectively designated as S1 peak, S2 peak, and RSD was calculated by calculating the relative retention time and the relative peak area, and the results are shown in tables 6 and 7 below.
The results showed that the RSD values for both relative retention time and relative peak area were less than 3%, indicating good reproducibility of the construction method.
TABLE 6 repeatability results (relative retention time)
TABLE 7 repeatability results (relative peak area)
(4) Stability investigation:
the same sample solutions as in example 2 were sampled and analyzed at 0, 4, 8, 12, 16, 20 and 24 hours, respectively, peak 1, peak 2, peak 4 and peak 5 were S1 peak with peak 3, peak 8 and peak 9 were S2 peak with peak 7, and relative retention time and relative peak area were calculated, and RSD were calculated, and the results are shown in tables 8 and 9.
The results showed that the RSD values for both the relative retention time and the relative peak area were less than 3%, indicating good durability of the construction method.
TABLE 8 stability results (relative retention time)
TABLE 9 stability results (relative peak area)
(5) Durability inspection
① Inspection of liquid chromatography instruments
The same sample solution in example 2 was taken and analyzed by two different liquid chromatographs, waters Acquity UPLC and Agilent Technologies 1290, respectively, of the Infinicity ultra-high performance liquid chromatograph, and the results are shown in FIG. 5.
The results show that the separation effect is better in two different chromatographs, indicating that the durability of the different instruments of the method is good.
② Inspection of chromatographic columns:
The same sample solution as in example 2 was taken and analyzed by selecting the following 3 chromatographic columns ：ACQUITY BEH C18(Waters,100×2.1mm,1.8μm)、ZORBAX Eclipse Plus C18(Agilent,100×2.1mm,1.8μm)、ZORBAX SB-C18 RRHD(Agilent,100×2.1mm,1.8μm), respectively, as shown in fig. 6.
The results showed that the chromatographic separation was better with 3 types of columns, indicating better durability of the different columns of the method, preferably column ZORBAX Eclipse Plus C (Agilent, 100X 2.1mm,1.8 μm).
③ Investigation of flow Rate
Taking the same sample solution in example 2, respectively examining the sample separation effect at the column temperature of 20 ℃ and 25 ℃ and 35 ℃, as shown in figure 7, the analysis method can obtain better separation of the hyperforin sample at the column temperature of 20 ℃ to 30 ℃ and can meet the requirement of system applicability with smaller column temperature variation. Preferably the column temperature is 25 ℃.
④ Investigation of column temperature
Taking the same sample solution in the embodiment 2, respectively examining the sample separation effect when the flow rates are 0.20ml/min, 0.25ml/min and 0.35ml/min, and as shown in figure 8, the hyperforin sample can be better separated when the flow rate is 0.20 ml/min-0.35 ml/min, and the system applicability requirement can be met by smaller flow rate fluctuation, and the durability is better. Preferably, the column temperature is 0.25ml/min.
Example 4
The quality control method of the standard decoction and the formula granule of the hypericum perforatum is applied to the identification of the formula granule of the hypericum perforatum and the pseudo-origanum standard decoction thereof, and is shown in figure 9.
Oregano and Hypericum perforatum prepared into standard decoction lose the original properties of decoction pieces and are difficult to identify singly. By adopting the method, the characteristic patterns of the two are compared with a very obvious difference, and other characteristic peaks except for the peak 1 hardly exist in the oregano standard decoction. In supervision, the method can help to judge whether the production raw materials of the hyperforin herb formula particles have errors.
Claims (6)
1. A quality detection method of hypericum perforatum standard decoction and formula particles is characterized by comprising the following steps: preparing a sample solution of Hypericum perforatum, preparing a reference substance solution of a reference substance, and obtaining a characteristic map of the sample solution by adopting an ultra-high performance liquid chromatography; the characteristic spectrum at least comprises 11 characteristic peaks including protocatechuic acid, neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, rutin, hyperoside, isoquercitrin, quercitrin and quercetin; the preparation process of the sample solution comprises the following steps: taking a test sample, adding a solvent, uniformly mixing, sealing, weighing, carrying out ultrasonic treatment, cooling, weighing again, supplementing the reduced weight with the solvent, shaking uniformly, and filtering to obtain a filtrate, wherein the filtrate is a test sample solution, and the solvent is a methanol aqueous solution with the mass concentration of 30% -70% or an ethanol aqueous solution with the mass concentration of 30% -75%; wherein the chromatographic conditions of the ultra-high performance liquid chromatography are as follows: chromatographic column: chromatographic column with octadecylsilane chemically bonded silica as filler; the detection wavelength is 300nm, acetonitrile is taken as a mobile phase A, 0.01% phosphoric acid solution is taken as a mobile phase B, and elution is carried out according to the following gradient elution program:
2. The method for detecting the quality of the standard decoction and the formula particles of the hypericum perforatum according to claim 1, wherein the reference substance solution of the reference substance is prepared by the following steps: taking a hyperin reference substance and a chlorogenic acid reference substance, precisely weighing, and respectively adding methanol to prepare solutions containing 10-100 mug of hyperin and 5-50 mug of chlorogenic acid per 1ml of the solutions serving as reference substance solutions of the reference substances.
3. The method for detecting the quality of the standard hyperforin decoction and the formula particles according to claim 1, wherein the mass-volume ratio of the test sample to the solvent is 0.1-0.5 g: 25-100 ml.
4. The method for detecting the quality of the standard decoction and the formula particles of hypericum perforatum according to claim 1, wherein the power of the ultrasonic treatment is 250-300W, the frequency is 40kHz, and the ultrasonic treatment time is 15-60min.
5. The method for detecting the quality of the standard decoction and the formula particles of the hypericum perforatum according to claim 1, wherein the sample injection volume of the reference substance solution is 1-5 mu L, and the sample injection volume of the sample solution is 1-5 mu L.
6. The use of the quality detection method of standard decoction and formulation of Hypericum perforatum according to claim 1 for distinguishing Hypericum perforatum from Oregano pseudostellaria.
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