CN113686724A - Extract determination method capable of shortening detection time - Google Patents
Extract determination method capable of shortening detection time Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 40
- 239000000284 extract Substances 0.000 title claims description 49
- 238000001514 detection method Methods 0.000 title description 11
- 238000004904 shortening Methods 0.000 title description 4
- 238000005303 weighing Methods 0.000 claims abstract description 113
- 238000001704 evaporation Methods 0.000 claims abstract description 92
- 238000001816 cooling Methods 0.000 claims abstract description 58
- 239000002904 solvent Substances 0.000 claims abstract description 41
- 239000003814 drug Substances 0.000 claims abstract description 22
- 238000010992 reflux Methods 0.000 claims abstract description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 110
- 238000001035 drying Methods 0.000 claims description 102
- 238000010438 heat treatment Methods 0.000 claims description 55
- 239000000706 filtrate Substances 0.000 claims description 47
- 238000001914 filtration Methods 0.000 claims description 36
- 230000008020 evaporation Effects 0.000 claims description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 238000009835 boiling Methods 0.000 claims description 19
- 238000007789 sealing Methods 0.000 claims description 19
- 239000007788 liquid Substances 0.000 claims description 18
- 238000000527 sonication Methods 0.000 claims description 3
- 239000000047 product Substances 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 235000008216 herbs Nutrition 0.000 claims 1
- 238000012360 testing method Methods 0.000 abstract description 54
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 238000007689 inspection Methods 0.000 abstract description 6
- 238000005259 measurement Methods 0.000 abstract description 3
- 238000012827 research and development Methods 0.000 abstract description 3
- 230000003631 expected effect Effects 0.000 abstract description 2
- 244000227573 Desmodium styracifolium Species 0.000 description 17
- 241001598107 Imperata Species 0.000 description 17
- 240000000249 Morus alba Species 0.000 description 17
- 235000008708 Morus alba Nutrition 0.000 description 17
- 230000001502 supplementing effect Effects 0.000 description 16
- 230000004580 weight loss Effects 0.000 description 16
- 238000009210 therapy by ultrasound Methods 0.000 description 14
- 240000006509 Gynostemma pentaphyllum Species 0.000 description 13
- 235000002956 Gynostemma pentaphyllum Nutrition 0.000 description 13
- 240000001659 Oldenlandia diffusa Species 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 8
- 239000000843 powder Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- 241000157511 Oldenlandia Species 0.000 description 6
- 238000011160 research Methods 0.000 description 6
- 238000011161 development Methods 0.000 description 4
- 244000025254 Cannabis sativa Species 0.000 description 1
- 241000212941 Glehnia Species 0.000 description 1
- 241000533388 Hansenia weberbaueriana Species 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229940126680 traditional chinese medicines Drugs 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
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
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Abstract
本发明公开了一种缩短检验时间的浸出物测定方法，涉及中医药领域，包括，称取供试品；加溶剂；预处理：将装有供试品和溶剂的锥形瓶进行超声处理20min，之后将锥形瓶与回流冷凝管连接；加热回流1h；自然冷却；补重；过滤；蒸发皿称重；干燥：将25ml滤液置于已干燥至恒重的蒸发皿中，水浴蒸干后，115℃烘干1h，置于干燥器中冷却30分钟，迅速称定重量；测定法：以干燥品计算供试品浸出物结果。本发明提出的方法在测定结果上与与药典方法检验结果一致，能够达到预期效果，同时很大程度上缩短检验时间，提升检验效率，降低研发、生产的时间成本。
The invention discloses a method for measuring leachate with shortened inspection time, which relates to the field of traditional Chinese medicine and includes: weighing a test sample; adding a solvent; pretreatment: ultrasonically treating a conical flask containing the test sample and the solvent for 20 minutes , then connect the conical flask to the reflux condenser; heat under reflux for 1 h; natural cooling; add weight; filter; weigh in an evaporating dish; , dried at 115 ℃ for 1h, placed in a desiccator for cooling for 30 minutes, and quickly weighed. The method proposed by the invention is consistent with the test results of the pharmacopoeia method in measurement results, can achieve the expected effect, and at the same time greatly shorten the test time, improve the test efficiency, and reduce the time cost of research and development and production.
Description
Technical Field
The invention relates to the field of traditional Chinese medicines, in particular to a method for measuring extract, which shortens the inspection time.
Background
The extract determination refers to determination of soluble substances in Chinese medicinal materials and decoction pieces with water or other suitable solvent. The method is mainly used for quality judgment of the following situations of the traditional Chinese medicine, the traditional Chinese medicine decoction pieces and the traditional Chinese medicine formula granules: 1. the active or index ingredient is unclear; 2. the content is very low; 3. there is no more precise method of quantification; 4. other detection means are used together.
The extract determination method is specified in the general rules 2201 of the four departments in the 2020 edition of Chinese pharmacopoeia:
the hot dipping method comprises the steps of taking about 2-4 g of a sample, precisely weighing, placing the sample in a 100-250 ml conical flask, precisely adding 50-100 ml of water, sealing, weighing, standing for 1 hour, connecting a reflux condensation pipe, heating to boil, and keeping slightly boiling for 1 hour. After cooling, the flask was taken off, the stopper was sealed, the weight was weighed again, the weight lost was made up with water, shaken well, filtered through a drying filter, 25ml of the filtrate was measured precisely, placed in an evaporation dish dried to constant weight, dried on a water bath, dried at 105 ℃ for 3 hours, placed in a desiccator for cooling for 30 minutes, and the weight was weighed precisely and quickly. The content (%) of the water-soluble extract in the test sample was calculated on a dry basis, unless otherwise specified.
Alcohol-soluble extract assay: measured according to the water-soluble extract measuring method. Except for other provisions, ethanol with the specified concentration under various varieties is used as a solvent instead of water.
The detection time of the detection method needs about 7 hours, and the next step of research or production can be carried out only after the extract detection result needs to be obtained in the research, development and production processes, so that more time is wasted, the detection progress is influenced, and the time cost of research, development and production is increased.
Disclosure of Invention
In order to solve the technical problems, the technical scheme provides the extract determination method for shortening the detection time, and solves the problems that the detection time of the traditional determination method provided in the background technology needs about 7 hours, the extract detection result needs to be obtained in the research, development and production processes, the next research or production can be carried out, the time is wasted, the detection progress is influenced greatly, and the time cost of research, development and production is increased.
In order to achieve the above purposes, the technical scheme adopted by the invention is as follows:
a method for measuring an extract with a shortened examination time, comprising the steps of:
weighing the following raw materials: weighing a sample to be measured with the weight of m1, and placing the sample in a 100ml conical flask;
adding a solvent: adding 50ml of ethanol into the conical flask, sealing the conical flask, and weighing the conical flask as m 2;
pretreatment: fully contacting a sample with a solvent, and then connecting the conical flask with a reflux condenser pipe;
heating: heating the conical flask until the ethanol in the conical flask boils, and keeping slight boiling for 1 hour;
and (3) natural cooling: taking down the conical flask, cooling the conical flask to room temperature, and weighing m 3;
and (3) complementing: adding ethanol m2-m3 into the conical flask, and shaking up;
and (3) filtering: filtering the liquid medicine in the conical flask by using a drying filter, and precisely measuring 25ml of filtrate;
weighing an evaporation dish: drying the evaporating dish to constant weight, and weighing m 4;
and (3) drying: placing 25ml of filtrate in an evaporating dish which is dried to constant weight, drying the filtrate in a water bath, placing the evaporating dish in a dryer, heating to 115 ℃, drying for 1 hour, placing the evaporating dish in the dryer, cooling for 30 minutes, and quickly weighing m 5;
the determination method comprises the following steps: the extract was calculated from the dried product.
Preferably, m1 is 2 g.
Preferably, the step of pretreatment is any one of standing for 1 hour or ultrasonic treatment for 20 min.
Further preferably, the step of pre-treatment is sonication for 20 min.
Preferably, the content of the water-soluble extract of the medicinal material is calculated in a mode of
Compared with the prior art, the invention has the advantages that:
the invention adopts the step of carrying out ultrasonic treatment on the conical flask filled with the medicinal materials and the solvent for 20min to replace standing for 1 hour, and simultaneously adopts drying at 115 ℃ for 1 hour to replace drying at 105 ℃ for 3 hours, thereby effectively reducing the inspection time, improving the inspection efficiency, shortening the drying time from the original 3 hours to 1 hour, reducing the use time of an oven, reducing the energy consumption of a laboratory, effectively reducing the overall inspection time, accelerating the inspection progress, and reducing the time cost of research and development and production.
Drawings
FIG. 1 is a schematic flow chart of the present invention.
Detailed Description
The following description is presented to disclose the invention so as to enable any person skilled in the art to practice the invention. The preferred embodiments in the following description are given by way of example only, and other obvious variations will occur to those skilled in the art.
Example one
Glehnia root extract powder extract
Taking 3 batches of radix glehniae as radix glehniae 1, radix glehniae 2 and radix glehniae 3 respectively;
weighing a test sample: weighing 2g of radix glehniae 1, radix glehniae 2 and radix glehniae 3 to be respectively placed in 100ml conical bottles;
adding a solvent: respectively adding 50ml of ethanol into the conical flasks, sealing the conical flasks, and weighing;
pretreatment: carrying out ultrasonic treatment on the conical flask filled with the test sample and the solvent for 20min, and then connecting the conical flask with a reflux condenser pipe;
heating: heating the conical flask until the ethanol in the conical flask boils, and keeping slight boiling for 1 hour;
and (3) natural cooling: taking down the conical flask, and naturally cooling the conical flask to room temperature;
and (3) complementing: supplementing the weight loss with ethanol, and shaking;
and (3) filtering: filtering the liquid medicine in the conical flask by using a drying filter, and precisely measuring 25ml of filtrate;
weighing an evaporation dish: drying the evaporating dish to constant weight, and weighing;
and (3) drying: placing 25ml of filtrate in an evaporating dish which is dried to constant weight, drying the filtrate in a water bath, placing the evaporating dish in a drying box, heating to 105 ℃, drying for 3 hours, placing the evaporating dish in a dryer, cooling for 30 minutes, and quickly weighing;
the determination method comprises the following steps: and calculating the extract results of the test sample, and marking the final results as 1-1 of radix glehniae, 2-1 of radix glehniae and 3-1 of radix glehniae.
Example two
Extract of radix Curcumae extract powder
Taking 3 batches of radix curcumae, respectively marking as radix curcumae 1, radix curcumae 2 and radix curcumae 3;
weighing a test sample: weighing 2g of radix curcumae 1, 2g of radix curcumae and 3 g of radix curcumae, and respectively placing the two into a 100ml conical flask;
adding a solvent: respectively adding 50ml of ethanol into the conical flasks, sealing the conical flasks, and weighing;
pretreatment: carrying out ultrasonic treatment on the conical flask filled with the test sample and the solvent for 20min, and then connecting the conical flask with a reflux condenser pipe;
heating: heating the conical flask until the ethanol in the conical flask boils, and keeping slight boiling for 1 hour;
and (3) natural cooling: taking down the conical flask, and naturally cooling the conical flask to room temperature;
and (3) complementing: supplementing the weight loss with ethanol, and shaking;
and (3) filtering: filtering the liquid medicine in the conical flask by using a drying filter, and precisely measuring 25ml of filtrate;
weighing an evaporation dish: drying the evaporating dish to constant weight, and weighing;
and (3) drying: placing 25ml of filtrate in an evaporating dish which is dried to constant weight, drying the filtrate in a water bath, placing the evaporating dish in a drying box, heating to 105 ℃, drying for 3 hours, placing the evaporating dish in a dryer, cooling for 30 minutes, and quickly weighing;
the determination method comprises the following steps: calculating the extract results of the test sample, and marking the final results as 1-1, 2-1 and 3-1 of radix curcumae.
EXAMPLE III
Extract of Notopterygium Incisum Ting extract powder
Taking 3 batches of notopterygium root and marking as notopterygium root 1, notopterygium root 2 and notopterygium root 3 respectively;
weighing a test sample: weighing 2g of notopterygium root 1, notopterygium root 2 and notopterygium root 3, and placing in 100ml conical bottles respectively;
adding a solvent: respectively adding 50ml of ethanol into the conical flasks, sealing the conical flasks, and weighing;
pretreatment: carrying out ultrasonic treatment on the conical flask filled with the test sample and the solvent for 20min, and then connecting the conical flask with a reflux condenser pipe;
heating: heating the conical flask until the ethanol in the conical flask boils, and keeping slight boiling for 1 hour;
and (3) natural cooling: taking down the conical flask, and naturally cooling the conical flask to room temperature;
and (3) complementing: supplementing the weight loss with ethanol, and shaking;
and (3) filtering: filtering the liquid medicine in the conical flask by using a drying filter, and precisely measuring 25ml of filtrate;
weighing an evaporation dish: drying the evaporating dish to constant weight, and weighing;
and (3) drying: placing 25ml of filtrate in an evaporating dish which is dried to constant weight, drying the filtrate in a water bath, placing the evaporating dish in a drying box, heating to 105 ℃, drying for 3 hours, placing the evaporating dish in a dryer, cooling for 30 minutes, and quickly weighing;
the determination method comprises the following steps: and calculating the results of the test article extracts, and marking the final results as notopterygium root 1-1, notopterygium root 2-1 and notopterygium root 3-1.
Example four
Extract powder extract of spreading hedyotis herb
Taking 3 batches of spreading hedyotis herb and respectively recording the spreading hedyotis herb as spreading hedyotis herb 1, spreading hedyotis herb 2 and spreading hedyotis herb 3;
weighing a test sample: weighing 2g of oldenlandia 1, oldenlandia 2 and oldenlandia 3, and placing in a 100ml conical flask respectively;
adding a solvent: respectively adding 50ml of ethanol into the conical flasks, sealing the conical flasks, and weighing;
pretreatment: carrying out ultrasonic treatment on the conical flask filled with the test sample and the solvent for 20min, and then connecting the conical flask with a reflux condenser pipe;
heating: heating the conical flask until the ethanol in the conical flask boils, and keeping slight boiling for 1 hour;
and (3) natural cooling: taking down the conical flask, and naturally cooling the conical flask to room temperature;
and (3) complementing: supplementing the weight loss with ethanol, and shaking;
and (3) filtering: filtering the liquid medicine in the conical flask by using a drying filter, and precisely measuring 25ml of filtrate;
weighing an evaporation dish: drying the evaporating dish to constant weight, and weighing;
and (3) drying: placing 25ml of filtrate in an evaporating dish which is dried to constant weight, drying the filtrate in a water bath, placing the evaporating dish in a drying box, heating to 105 ℃, drying for 3 hours, placing the evaporating dish in a dryer, cooling for 30 minutes, and quickly weighing;
the determination method comprises the following steps: and calculating the extract results of the test sample, and marking the final results as 1-1 part of spreading hedyotis herb, 2-1 part of spreading hedyotis herb and 3-1 part of spreading hedyotis herb.
EXAMPLE five
Extract of mulberry leaf extract powder
Taking 3 batches of mulberry leaves, respectively marking as mulberry leaves 1, 2 and 3;
weighing a test sample: weighing 2g of to-be-treated mulberry leaves 1, 2g of mulberry leaves and 3 g of mulberry leaves, and respectively placing the to-be-treated mulberry leaves in a 100ml conical flask;
adding a solvent: respectively adding 50ml of ethanol into the conical flasks, sealing the conical flasks, and weighing;
pretreatment: standing the conical flask filled with the sample and the solvent for 1h, and then connecting the conical flask with a reflux condenser pipe;
heating: heating the conical flask until the ethanol in the conical flask boils, and keeping slight boiling for 1 hour;
and (3) natural cooling: taking down the conical flask, and naturally cooling the conical flask to room temperature;
and (3) complementing: supplementing the weight loss with ethanol, and shaking;
and (3) filtering: filtering the liquid medicine in the conical flask by using a drying filter, and precisely measuring 25ml of filtrate;
weighing an evaporation dish: drying the evaporating dish to constant weight, and weighing;
and (3) drying: placing 25ml of filtrate in an evaporating dish which is dried to constant weight, drying the filtrate in a water bath, placing the evaporating dish in a drying box, heating to 115 ℃, drying for 1 hour, placing the evaporating dish in a dryer, cooling for 30 minutes, and quickly weighing;
the determination method comprises the following steps: and calculating the result of the test article extract, and recording the final result as mulberry leaf 1-1, mulberry leaf 2-1 and mulberry leaf 3-1.
EXAMPLE six
Extract of Gynostemma pentaphyllum extract powder
Taking 3 batches of gynostemma pentaphylla, respectively marking as gynostemma pentaphylla 1, gynostemma pentaphylla 2 and gynostemma pentaphylla 3;
weighing a test sample: weighing 2g of gynostemma pentaphylla 1, 2 and 3, and respectively placing in a 100ml conical flask;
adding a solvent: respectively adding 50ml of ethanol into the conical flasks, sealing the conical flasks, and weighing;
pretreatment: pretreatment: standing the conical flask filled with the sample and the solvent for 1h, and then connecting the conical flask with a reflux condenser pipe;
heating: heating the conical flask until the ethanol in the conical flask boils, and keeping slight boiling for 1 hour;
and (3) natural cooling: taking down the conical flask, and naturally cooling the conical flask to room temperature;
and (3) complementing: supplementing the weight loss with ethanol, and shaking;
and (3) filtering: filtering the liquid medicine in the conical flask by using a drying filter, and precisely measuring 25ml of filtrate;
weighing an evaporation dish: drying the evaporating dish to constant weight, and weighing;
and (3) drying: placing 25ml of filtrate in an evaporating dish which is dried to constant weight, drying the filtrate in a water bath, placing the evaporating dish in a drying box, heating to 115 ℃, drying for 1 hour, placing the evaporating dish in a dryer, cooling for 30 minutes, and quickly weighing;
the determination method comprises the following steps: and calculating the result of the test article extract, and marking the final result as gynostemma pentaphylla 1-1, gynostemma pentaphylla 2-1 and gynostemma pentaphylla 3-1.
EXAMPLE seven
Desmodium styracifolium extract powder extract
Marking 3 batches of desmodium styracifolium as desmodium styracifolium 1, desmodium styracifolium 2 and desmodium styracifolium 3 respectively;
weighing a test sample: weighing 2g of desmodium styracifolium 1 to be treated, desmodium styracifolium 2 and desmodium styracifolium 3, and respectively placing the weighed materials in a 100ml conical flask;
adding a solvent: respectively adding 50ml of ethanol into the conical flasks, sealing the conical flasks, and weighing;
pretreatment: standing the conical flask filled with the sample and the solvent for 1h, and then connecting the conical flask with a reflux condenser pipe;
heating: heating the conical flask until the ethanol in the conical flask boils, and keeping slight boiling for 1 hour;
and (3) natural cooling: taking down the conical flask, and naturally cooling the conical flask to room temperature;
and (3) complementing: supplementing the weight loss with ethanol, and shaking;
and (3) filtering: filtering the liquid medicine in the conical flask by using a drying filter, and precisely measuring 25ml of filtrate;
weighing an evaporation dish: drying the evaporating dish to constant weight, and weighing;
and (3) drying: placing 25ml of filtrate in an evaporating dish which is dried to constant weight, drying the filtrate in a water bath, placing the evaporating dish in a drying box, heating to 115 ℃, drying for 1 hour, placing the evaporating dish in a dryer, cooling for 30 minutes, and quickly weighing;
the determination method comprises the following steps: and calculating the extract results of the test sample, and recording the final results as 1-1 part of desmodium styracifolium, 2-1 part of desmodium styracifolium and 3-1 part of desmodium styracifolium.
Example eight
Extract of lalang grass rhizome extract powder
Taking 3 batches of cogongrass rhizome, respectively marking as cogongrass rhizome 1, cogongrass rhizome 2 and cogongrass rhizome 3;
weighing a test sample: weighing 4g of cogongrass rhizome to be treated 1, cogongrass rhizome 2 and cogongrass rhizome 3, and respectively placing the materials in a 100ml conical flask;
adding a solvent: respectively adding 50ml of ethanol into the conical flasks, sealing the conical flasks, and weighing;
pretreatment: carrying out ultrasonic treatment on the conical flask filled with the test sample and the solvent for 20min, and then connecting the conical flask with a reflux condenser pipe;
heating: heating the conical flask until the ethanol in the conical flask boils, and keeping slight boiling for 1 hour;
and (3) natural cooling: taking down the conical flask, and naturally cooling the conical flask to room temperature;
and (3) complementing: supplementing the weight loss with ethanol, and shaking;
and (3) filtering: filtering the liquid medicine in the conical flask by using a drying filter, and precisely measuring 25ml of filtrate;
weighing an evaporation dish: drying the evaporating dish to constant weight, and weighing;
and (3) drying: placing 25ml of filtrate in an evaporating dish which is dried to constant weight, drying the filtrate in a water bath, placing the evaporating dish in a drying box, heating to 115 ℃, drying for 1 hour, placing the evaporating dish in a dryer, cooling for 30 minutes, and quickly weighing;
the determination method comprises the following steps: and calculating the result of the extract of the test sample, and marking the final result as 1-1 part of cogongrass rhizome, 2-1 part of cogongrass rhizome and 3-1 part of cogongrass rhizome.
Comparative example 1
Weighing a test sample: weighing 2g of radix glehniae 1, radix glehniae 2 and radix glehniae 3 to be respectively placed in 100ml conical bottles;
adding a solvent: respectively adding 50ml of ethanol into a 100ml conical flask, sealing the conical flask, and weighing;
standing: standing the conical flask filled with the test sample and the solvent for 1 hour, and then connecting the conical flask with a reflux condenser pipe;
heating: heating the conical flask until the ethanol in the conical flask boils, and keeping slight boiling for 1 hour;
and (3) natural cooling: taking down the conical flask, and naturally cooling the conical flask to room temperature;
and (3) complementing: supplementing the weight loss with ethanol, and shaking;
and (3) filtering: filtering the liquid medicine in the conical flask by using a drying filter, and precisely measuring 25ml of filtrate;
weighing an evaporation dish: drying the evaporating dish to constant weight, and weighing;
and (3) drying: placing 25ml of filtrate in an evaporating dish which is dried to constant weight, drying by evaporation in a water bath, placing the evaporating dish in a dryer, heating to 105 ℃, drying for 3 hours, placing in the dryer, cooling for 30 minutes, and quickly weighing;
the determination method comprises the following steps: and calculating the extract results of the test sample, and marking the final results as 1-2 parts of radix glehniae, 2-2 parts of radix glehniae and 3-2 parts of radix glehniae.
Comparative example No. two
Weighing a test sample: weighing 2g of radix curcumae 1, 2g of radix curcumae and 3 g of radix curcumae, and respectively placing the two into a 100ml conical flask;
adding a solvent: respectively adding 50ml of ethanol into a 100ml conical flask, sealing the conical flask, and weighing;
ultrasonic treatment: standing the conical flask filled with the test sample and the solvent for 1 hour, and then connecting the conical flask with a reflux condenser pipe;
heating: heating the conical flask until the ethanol in the conical flask boils, and keeping slight boiling for 1 hour;
and (3) natural cooling: taking down the conical flask, and naturally cooling the conical flask to room temperature;
and (3) complementing: supplementing the weight loss with ethanol, and shaking;
and (3) filtering: filtering the liquid medicine in the conical flask by using a drying filter, and precisely measuring 25ml of filtrate;
weighing an evaporation dish: drying the evaporating dish to constant weight, and weighing;
and (3) drying: placing 25ml of filtrate in an evaporating dish which is dried to constant weight, drying by evaporation in a water bath, placing the evaporating dish in a dryer, heating to 105 ℃, drying for 3 hours, placing in the dryer, cooling for 30 minutes, and quickly weighing;
the determination method comprises the following steps: and calculating the extract results of the test sample, and marking the final results as 1-2 parts of radix curcumae, 2-2 parts of radix curcumae and 3-2 parts of radix curcumae.
Comparative example No. three
Weighing a test sample: weighing 2g of notopterygium root 1, notopterygium root 2 and notopterygium root 3, and placing in 100ml conical bottles respectively;
adding a solvent: respectively adding 50ml of ethanol into a 100ml conical flask, sealing the conical flask, and weighing;
ultrasonic treatment: standing the conical flask filled with the test sample and the solvent for 1 hour, and then connecting the conical flask with a reflux condenser pipe;
heating: heating the conical flask until the ethanol in the conical flask boils, and keeping slight boiling for 1 hour;
and (3) natural cooling: taking down the conical flask, and naturally cooling the conical flask to room temperature;
and (3) complementing: supplementing the weight loss with ethanol, and shaking;
and (3) filtering: filtering the liquid medicine in the conical flask by using a drying filter, and precisely measuring 25ml of filtrate;
weighing an evaporation dish: drying the evaporating dish to constant weight, and weighing;
and (3) drying: placing 25ml of filtrate in an evaporating dish which is dried to constant weight, drying by evaporation in a water bath, placing the evaporating dish in a dryer, heating to 105 ℃, drying for 3 hours, placing in the dryer, cooling for 30 minutes, and quickly weighing;
the determination method comprises the following steps: and calculating the results of the test article extracts, and marking the final results as notopterygium root 1-2, notopterygium root 2-2 and notopterygium root 3-2.
Comparative example No. four
Weighing a test sample: weighing 2g of oldenlandia 1, oldenlandia 2 and oldenlandia 3, and placing in a 100ml conical flask respectively;
adding a solvent: respectively adding 50ml of ethanol into a 100ml conical flask, sealing the conical flask, and weighing;
ultrasonic treatment: standing the conical flask filled with the test sample and the solvent for 1 hour, and then connecting the conical flask with a reflux condenser pipe;
heating: heating the conical flask until the ethanol in the conical flask boils, and keeping slight boiling for 1 hour;
and (3) natural cooling: taking down the conical flask, and naturally cooling the conical flask to room temperature;
and (3) complementing: supplementing the weight loss with ethanol, and shaking;
and (3) filtering: filtering the liquid medicine in the conical flask by using a drying filter, and precisely measuring 25ml of filtrate;
weighing an evaporation dish: drying the evaporating dish to constant weight, and weighing;
and (3) drying: placing 25ml of filtrate in an evaporating dish which is dried to constant weight, drying by evaporation in a water bath, placing the evaporating dish in a dryer, heating to 105 ℃, drying for 3 hours, placing in the dryer, cooling for 30 minutes, and quickly weighing;
the determination method comprises the following steps: and calculating the extract results of the test sample, and marking the final results as 1-2 parts of oldenlandia diffusa, 2-2 parts of oldenlandia diffusa and 3-2 parts of oldenlandia diffusa.
Comparative example five
Weighing a test sample: weighing 2g of to-be-treated mulberry leaves 1, 2g of mulberry leaves and 3 g of mulberry leaves, and respectively placing the to-be-treated mulberry leaves in a 100ml conical flask;
adding a solvent: respectively adding 50ml of ethanol into a 100ml conical flask, sealing the conical flask, and weighing;
ultrasonic treatment: standing the conical flask filled with the test sample and the solvent for 1 hour, and then connecting the conical flask with a reflux condenser pipe;
heating: heating the conical flask until the ethanol in the conical flask boils, and keeping slight boiling for 1 hour;
and (3) natural cooling: taking down the conical flask, and naturally cooling the conical flask to room temperature;
and (3) complementing: supplementing the weight loss with ethanol, and shaking;
and (3) filtering: filtering the liquid medicine in the conical flask by using a drying filter, and precisely measuring 25ml of filtrate;
weighing an evaporation dish: drying the evaporating dish to constant weight, and weighing;
and (3) drying: placing 25ml of filtrate in an evaporating dish which is dried to constant weight, drying by evaporation in a water bath, placing the evaporating dish in a dryer, heating to 105 ℃, drying for 3 hours, placing in the dryer, cooling for 30 minutes, and quickly weighing;
the determination method comprises the following steps: and calculating the result of the test article extract, and recording the final result as mulberry leaf 1-2, mulberry leaf 2-2 and mulberry leaf 3-2.
Comparative example six
Weighing a test sample: weighing 2g of gynostemma pentaphylla 1, 2 and 3, and respectively placing in a 100ml conical flask;
adding a solvent: respectively adding 50ml of ethanol into a 100ml conical flask, sealing the conical flask, and weighing;
ultrasonic treatment: standing the conical flask filled with the test sample and the solvent for 1 hour, and then connecting the conical flask with a reflux condenser pipe;
heating: heating the conical flask until the ethanol in the conical flask boils, and keeping slight boiling for 1 hour;
and (3) natural cooling: taking down the conical flask, and naturally cooling the conical flask to room temperature;
and (3) complementing: supplementing the weight loss with ethanol, and shaking;
and (3) filtering: filtering the liquid medicine in the conical flask by using a drying filter, and precisely measuring 25ml of filtrate;
weighing an evaporation dish: drying the evaporating dish to constant weight, and weighing;
and (3) drying: placing 25ml of filtrate in an evaporating dish which is dried to constant weight, drying by evaporation in a water bath, placing the evaporating dish in a dryer, heating to 105 ℃, drying for 3 hours, placing in the dryer, cooling for 30 minutes, and quickly weighing;
the determination method comprises the following steps: and calculating the result of the test article extract, and marking the final result as gynostemma pentaphylla 1-2, gynostemma pentaphylla 2-2 and gynostemma pentaphylla 3-2.
Comparative example seven
Weighing a test sample: weighing 2g of desmodium styracifolium 1 to be treated, desmodium styracifolium 2 and desmodium styracifolium 3, and respectively placing the weighed materials in a 100ml conical flask;
adding a solvent: respectively adding 50ml of ethanol into a 100ml conical flask, sealing the conical flask, and weighing;
ultrasonic treatment: standing the conical flask filled with the test sample and the solvent for 1 hour, and then connecting the conical flask with a reflux condenser pipe;
heating: heating the conical flask until the ethanol in the conical flask boils, and keeping slight boiling for 1 hour;
and (3) natural cooling: taking down the conical flask, and naturally cooling the conical flask to room temperature;
and (3) complementing: supplementing the weight loss with ethanol, and shaking;
and (3) filtering: filtering the liquid medicine in the conical flask by using a drying filter, and precisely measuring 25ml of filtrate;
weighing an evaporation dish: drying the evaporating dish to constant weight, and weighing;
and (3) drying: placing 25ml of filtrate in an evaporating dish which is dried to constant weight, drying by evaporation in a water bath, placing the evaporating dish in a dryer, heating to 105 ℃, drying for 3 hours, placing in the dryer, cooling for 30 minutes, and quickly weighing;
the determination method comprises the following steps: and calculating the extract result of the test sample, and recording the final result as 1-2 parts of desmodium styracifolium, 2-2 parts of desmodium styracifolium and 3-2 parts of desmodium styracifolium.
Comparative example eight
Weighing a test sample: weighing 2g of cogongrass rhizome to be treated 1, cogongrass rhizome 2 and cogongrass rhizome 3, and respectively placing the materials in a 100ml conical flask;
adding a solvent: respectively adding 50ml of ethanol into a 100ml conical flask, sealing the conical flask, and weighing;
ultrasonic treatment: standing the conical flask filled with the test sample and the solvent for 1 hour, and then connecting the conical flask with a reflux condenser pipe;
heating: heating the conical flask until the ethanol in the conical flask boils, and keeping slight boiling for 1 hour;
and (3) natural cooling: taking down the conical flask, and naturally cooling the conical flask to room temperature;
and (3) complementing: supplementing the weight loss with ethanol, and shaking;
and (3) filtering: filtering the liquid medicine in the conical flask by using a drying filter, and precisely measuring 25ml of filtrate;
weighing an evaporation dish: drying the evaporating dish to constant weight, and weighing;
and (3) drying: placing 25ml of filtrate in an evaporating dish which is dried to constant weight, drying by evaporation in a water bath, placing the evaporating dish in a dryer, heating to 105 ℃, drying for 3 hours, placing in the dryer, cooling for 30 minutes, and quickly weighing;
the determination method comprises the following steps: and calculating the result of the extract of the test sample, and marking the final result as 1-2 parts of cogongrass rhizome, 2-2 parts of cogongrass rhizome and 3-2 parts of cogongrass rhizome.
The results of the content measurement are as follows
Wherein RD represents the difference between different times of the same method in the same batch, and RSD represents the measured difference between different methods used in the same sample batch, wherein RD is required to be less than or equal to 5%, and RSD is required to be less than or equal to 5%.
The result shows that the method provided by the invention is consistent with the test result of the pharmacopoeia method in the measurement result, can achieve the expected effect, and simultaneously shortens the test time to a great extent, improves the test efficiency, and reduces the time cost of research and development and production.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are merely illustrative of the principles of the invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (5)
1. A method for measuring an extract with a shortened examination time, comprising the steps of:
weighing the following raw materials: weighing a sample to be measured with the weight of m1, and placing the sample in a conical flask of 100 ml;
adding a solvent: adding 50ml of ethanol into the conical flask, sealing the conical flask, and weighing the conical flask as m 2;
pretreatment: fully contacting a sample with a solvent, and then connecting the conical flask with a reflux condenser pipe;
heating: heating the conical flask until the ethanol in the conical flask boils, and keeping slight boiling for 1 hour;
and (3) natural cooling: taking down the conical flask, cooling the conical flask to room temperature, and weighing m 3;
and (3) complementing: adding ethanol with the weight of m2-m3 into the conical flask, and shaking up;
and (3) filtering: filtering the liquid medicine in the conical flask by using a drying filter, and precisely measuring 25ml of filtrate;
weighing an evaporation dish: drying the evaporating dish to constant weight, and weighing m 4;
and (3) drying: placing 25ml of filtrate in an evaporating dish which is dried to constant weight, drying the filtrate in a water bath, placing the evaporating dish in a dryer, heating to 115 ℃, drying for 1 hour, placing the evaporating dish in the dryer, cooling for 30 minutes, and quickly weighing m 5;
the determination method comprises the following steps: the extract was calculated from the dried product.
2. The method for assaying leachate according to claim 1, wherein m1 is 2 g.
3. The method for assaying leachate according to claim 1, wherein the pretreatment step is either standing for 1 hour or sonication for 20 min.
4. The method for assaying leachate according to claim 3, wherein the step of pretreatment is sonication for 20 min.
5. The method as claimed in claim 1, wherein the content of water soluble extract of the herbs is calculated by
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