CN110873776B - Identification method of gardenia and fried gardenia formula granules - Google Patents
Identification method of gardenia and fried gardenia formula granules Download PDFInfo
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- CN110873776B CN110873776B CN201811006054.3A CN201811006054A CN110873776B CN 110873776 B CN110873776 B CN 110873776B CN 201811006054 A CN201811006054 A CN 201811006054A CN 110873776 B CN110873776 B CN 110873776B
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Abstract
The invention discloses a method for identifying gardenia and fried gardenia formula granules. The identification method of the gardenia and fried gardenia formula particles achieves the purpose of identifying the gardenia and the fried gardenia by observing whether fluorescent spots at the designated positions of a thin-layer chromatography spectrogram are colored or not. Compared with HPLC fingerprint comparison, the method is simpler, has shorter detection time and higher efficiency, reduces the detection cost and provides a new method for identifying the gardenia prescription preparation.
Description
Technical Field
The invention particularly relates to an identification method of gardenia and fried gardenia formula granules.
Background
Gardenia (Gradenia jasminoides Ellis) belongs to Gardenia plants of Rubiaceae, belongs to the first medical and edible dual-purpose resource issued by Ministry of health, is a traditional Chinese medicine, has the effects of protecting liver, promoting bile flow, reducing blood pressure, calming, stopping bleeding, reducing swelling and the like, and is commonly used for treating diseases such as jaundice type hepatitis, sprain and contusion, hypertension, diabetes and the like in traditional Chinese medicine clinical practice. The gardenia yellow pigment which takes crocin and crocin as main components is usually extracted from food.
A method for preparing parched fructus Gardeniae comprises parching clean fructus Gardeniae to brown, clearing pathogenic fire, relieving restlessness, clearing heat, promoting diuresis, cooling blood, and removing toxic substances. Can be used for treating vexation due to fever, jaundice, dark urine, stranguria with blood, pain, hematemesis, epistaxis, conjunctival congestion, swelling and pain, and pyocutaneous disease due to pathogenic fire; it can be used for treating sprain, contusion and pain. Raw gardenia is mainly used for purging fire, removing toxicity, promoting bile flow and removing jaundice, while fried gardenia is mainly used for clearing heat, relieving restlessness, cooling blood and stopping bleeding.
At present, the identification of gardenia and processed products thereof is mainly carried out through fingerprint comparison. For example, the fingerprint comparison of Baojia, Liuling, gardenia and processed products thereof [ J ] in China pharmaceutical industry journal, 2016.47(2), 163-. However, the HPLC method is long in use time, complex, basically consistent in overall picture and appearance, and low in efficiency in the actual application process.
Disclosure of Invention
In order to solve the problems, the invention provides a novel identification method of gardenia and fried gardenia formula granules.
The invention more particularly provides a thin-layer chromatography identification method of gardenia and fried gardenia formula particles, which adopts a thin-layer chromatography analysis method to identify the gardenia and the fried gardenia formula particles and comprises the following specific steps:
(1) extracting the medicines to be detected with petroleum ether, filtering, evaporating the filtrate, and dissolving the residue with chloroform to obtain sample solution;
(2) sucking a test sample solution for thin-layer chromatography detection, wherein the thin-layer plate is a silica gel G thin-layer plate, and a developing agent is cyclohexane-ethyl acetate;
(3) and (3) observing under an ultraviolet lamp, if blue fluorescent spots exist at the position of 0.144 +/-25 percent of Rf value, the fried gardenia medicinal material or the formula particle is obtained, and if blue fluorescent spots do not exist at the position of 0.144 +/-25 percent of Rf value, the fried gardenia medicinal material or the formula particle is obtained.
In the step (1), the mass volume ratio of the drug to be detected to the petroleum ether is 1g:50 ml.
In the step (1), the boiling point of the petroleum ether is 60-90 ℃.
In the step (1), the extraction is ultrasonic extraction; the extraction time is 30 min.
In the step (1), the mass volume ratio of the trichloromethane to the medicine to be detected is 1ml:1 g.
In the step (2), the sample amount is 10-20 μ l.
In the step (2), the ratio of cyclohexane to ethyl acetate is 7: 3.
in the step (3), the wavelength of the ultraviolet light is 365 nm.
In the step (3), the inspection is performed at a temperature of 4-25 ℃ and a humidity of 32-75%. In the step (3), the Rf value is 0.143.
The identification method of the gardenia and fried gardenia formula particles achieves the purpose of identifying the gardenia and the fried gardenia by observing whether fluorescent spots at the designated positions of a thin-layer chromatography spectrogram are colored or not. Compared with HPLC fingerprint comparison, the method is simpler, the detection time is shorter, the efficiency is higher, the detection cost is reduced, and a novel method with strong practicability is provided for identifying the gardenia formula preparation.
Obviously, many modifications, substitutions, and variations are possible in light of the above teachings of the invention, without departing from the basic technical spirit of the invention, as defined by the following claims.
The present invention will be described in further detail with reference to the following examples. This should not be understood as limiting the scope of the above-described subject matter of the present invention to the following examples. All the technologies realized based on the above contents of the present invention belong to the scope of the present invention.
Drawings
FIG. 1 shows the different quantitative sample results (1: 1. mu.l of fried gardenia prescription granule, 2: 3. mu.l of fried gardenia prescription granule, 3: 5. mu.l of fried gardenia prescription granule, 4: 10. mu.l of fried gardenia prescription granule, 5: 20. mu.l of fried gardenia prescription granule, 6: 1. mu.l of gardenia contrast medicinal material, 7: 3. mu.l of gardenia contrast medicinal material, 8: 5. mu.l of gardenia contrast medicinal material, 9: 10. mu.l of gardenia contrast medicinal material, 10: 20. mu.l of gardenia contrast medicinal material)
FIG. 2 thin layer chromatogram of parched fructus Gardeniae granule (1: parched fructus Gardeniae granule; 2: negative; 3: fructus Gardeniae control medicinal material)
FIG. 3 Qingdao sea wave silica gel G plate (1: fructus Gardeniae reference material; 2-4: parched fructus Gardeniae formula granule)
FIG. 4 shows Qingdao Yumin silica gel G plate (1: fructus Gardeniae reference material; 2-4: parched fructus Gardeniae formula granule)
FIG. 5 Qingdao sea silica gel G plate (1: fructus Gardeniae reference material; 2-4: parched fructus Gardeniae formula granule)
FIG. 6 thin-layer chromatogram of parched fructus Gardeniae formula granule at low temperature of 4 deg.C (1: fructus Gardeniae reference material; 2-4: parched fructus Gardeniae formula granule)
FIG. 7 thin layer chromatogram of parched fructus Gardeniae formula granule at room temperature and 4 deg.C (1: fructus Gardeniae reference material; 2-4: parched fructus Gardeniae formula granule)
FIG. 8 thin layer chromatogram of parched fructus Gardeniae formula granule with humidity of 32% (1: fructus Gardeniae reference material; 2-4: parched fructus Gardeniae formula granule)
FIG. 9 thin layer chromatogram of parched fructus Gardeniae formula granule with humidity of 75% (1: fructus Gardeniae reference material; 2-4: parched fructus Gardeniae formula granule)
FIG. 10 shows the thin-layer identification of the fructus Gardeniae, fructus Gardeniae preparata, and fructus Gardeniae preparata formula granules (1: fructus Gardeniae formula granule SY 1803004; 2: fructus Gardeniae formula granule SY 1803005; 3: fructus Gardeniae formula granule SY 1803006; 4: fructus Gardeniae preparata formula granule SY 1802001; 5: fructus Gardeniae preparata formula granule SY 1802002; 6: fructus Gardeniae preparata formula granule SY1802003)
Detailed Description
Example 1 identification method of raw and fried gardenia formulation granule of the present invention
Respectively taking fructus Gardeniae control material and fructus Gardeniae formula granule 1.0g, grinding, adding 50ml petroleum ether (60-90 deg.C), treating with ultrasound (power 250W, frequency 40kHz) for 30min, filtering, evaporating filtrate, and dissolving residue with 1ml chloroform to obtain sample solution. Performing thin layer chromatography (0502 of the four ministry of the ministry of China pharmacopoeia 2015), sucking 10-20 μ l of each of the two solutions, spotting on the same silica gel G thin layer plate, developing with cyclohexane-ethyl acetate (7: 3) as developing agent, taking out, air drying, inspecting under ultraviolet lamp (365nm), and determining that no blue fluorescent spot appears on the silica gel G thin layer plate with a specific migration value of 0.144 + -25% in the chromatogram of the sample, thereby determining the Gardenia jasminoides ellis formula granule.
Example 2 identification method of raw and fried gardenia formulation granule of the present invention
Respectively taking fructus Gardeniae control material and parched fructus Gardeniae granule 1.0g, grinding, adding 50ml petroleum ether (60-90 deg.C), treating with ultrasound (power 250W, frequency 40kHz) for 30min, filtering, evaporating filtrate to dryness, and dissolving residue with 1ml chloroform to obtain sample solution. Performing thin layer chromatography (0502 of the four ministerial rules of the science of Chinese pharmacopoeia 2015), sucking 10-20 μ l of each of the two solutions, dropping on the same silica gel G thin layer plate, developing with cyclohexane-ethyl acetate (7: 3) as developing agent, taking out, air drying, inspecting under an ultraviolet lamp (365nm), and displaying blue fluorescent spots on the silica gel G thin layer plate with a specific migration value of 0.144 +/-25% in the chromatogram of the sample to determine the fried gardenia formula particles.
The following test examples specifically illustrate the advantageous effects of the present invention:
test example 1 thin layer methodology examination
1. Laboratory apparatus and reagent
1.1 instruments
An ultrasonic cleaner: KQ5200DB model (600W, 40 KHz; ultrasonic instruments, Inc. of Kunshan), mortar, thin layer imaging System: CAMAG TLC Visualizer, silica gel G thin layer plate (Qingdao Seawaking plant, lot No. 180107, Tianjin Silida science and technology Co., Ltd., lot No. 170907, Qingdao Yumin plant, lot No. 180206).
1.2 reagents
Fructus Gardeniae control medicinal material (China food and drug inspection research institute, lot number: 120988-.
2 thin layer chromatography method investigation
Taking 1.0g of sample, grinding, adding 50ml of petroleum ether (60-90 ℃), treating with ultrasound (power 250W, frequency 40kHz) for 30 minutes, filtering, evaporating filtrate to dryness, and dissolving residue with 1ml of chloroform to obtain sample solution. Performing thin layer chromatography (0502 of the four parts of the pharmacopoeia of China 2015), sucking 10-20 μ l of each solution, dropping on the same silica gel G thin layer plate, developing with cyclohexane-ethyl acetate (7: 3) as developing agent, taking out, air drying, and inspecting under ultraviolet lamp (365 nm).
2.1 dot sample amount investigation
Under the above-defined experimental conditions, 1. mu.l, 3. mu.l, 5. mu.l, 10. mu.l and 20. mu.l of the control solution and the test solution were spotted on the same silica gel G thin layer plate, respectively, and the blue fluorescence spot shift value (Rf) at 1.5cm from the origin was 0.167, as shown in FIG. 1. As can be seen from the figure, when the control drug solution is spotted by 10-20 μ l, the sample solution to be tested is spotted by 10-20 μ l, the ideal effect can be achieved.
2.2 specialization examination
Preparing fructus Gardeniae control solution, parched fructus Gardeniae granule solution, and negative solution according to the above test preparation method, performing thin layer identification test, and obtaining a blue fluorescence spot shift value (Rf) of 0.170 at a distance of 1.7cm from the origin, with the result shown in FIG. 2. As can be seen from the figure, the method has better specificity.
2.3 investigation of durability
2.3.1 comparison of different lamella plates
Selecting a prefabricated silica gel G plate of a Qingdao ocean wave chemical plant branch, a cuttable thin-layer chromatography plate (silica gel G plate) of Tianjin Silida science and technology limited company, and a prefabricated silica gel G plate of a Qingdao Yumin chemical plant branch, and respectively testing according to a formulated test method, wherein the test methods are shown in figures 3-5. The results show that the blue fluorescence spot specific shift values (Rf) at 1-1.5cm from the origin in the three thin-layer plates are respectively 0.117, 0.122 and 0.143, and can meet the identification requirements.
2.3.2 comparison of different temperatures
And (3) taking the spotted thin-layer plate, and respectively developing the thin-layer plate at the low temperature of 4 ℃ and the normal temperature of 25 ℃. See FIGS. 6-7. As can be seen from the figure, the method has better adaptability to different temperatures, and the blue spot specific shift values (Rf) are 0.136 and 0.176 respectively.
2.3.3 comparison of different humidities
The spotted sheets were then spread in a humidity environment of 32% and 75%, respectively, as shown in FIGS. 8-9. As can be seen, the method has better adaptability to different humidities, and the blue spot specific shift values (Rf) are respectively 0.105 and 0.158.
2.4 authentication
The thin-layer identification of 9 batches of the gardenia, fried gardenia and scorched gardenia formula particles is verified, the blue fluorescence spot ratio shift value (Rf) at 1.2cm from the origin is 0.143, and the test result is shown in figure 10.
Determination of 2.5 Shift value (Rf)
The data of each ratio shift value inspected by the thin layer chromatography method are summarized in Table 1
TABLE 1 summary of the various shift values
According to the summary results, the following results are obtained: finally, it was determined that the specific shift value (Rf) of the spot should be within. + -. 25% of the specified value, which is 0.144.
The identification method of the gardenia and fried gardenia formula particles achieves the purpose of identifying the gardenia and the fried gardenia by observing whether fluorescent spots at the designated positions of a thin-layer chromatography spectrogram are colored or not. Compared with HPLC fingerprint comparison, the method is simpler, the detection time is shorter, the efficiency is higher, the detection cost is reduced, and a novel method with strong practicability is provided for identifying the gardenia formula preparation.
Claims (9)
1. A method for identifying gardenia and fried gardenia is characterized by comprising the following steps: identifying the gardenia and fried gardenia formula particles by adopting a thin-layer chromatography, and specifically comprising the following steps:
(1) extracting the medicines to be detected with petroleum ether, filtering, evaporating the filtrate, and dissolving the residue with chloroform to obtain sample solution;
(2) sucking a test sample solution for thin-layer chromatography detection, wherein the thin-layer plate is a silica gel G thin-layer plate, and a developing agent is cyclohexane-ethyl acetate; the cyclohexane-ethyl acetate ratio is 7: 3;
(3) and (3) observing under an ultraviolet lamp, wherein the fried gardenia formula particles are obtained if blue fluorescent spots exist at the position of 0.144 +/-25% of the Rf value, and the gardenia formula particles are obtained if blue fluorescent spots do not exist at the position of 0.144 +/-25% of the Rf value.
2. The authentication method according to claim 1, wherein: in the step (1), the mass volume ratio of the drug to be detected to the petroleum ether is 1g:50 ml.
3. The authentication method according to claim 1, wherein: in the step (1), the boiling point of the petroleum ether is 60-90 ℃.
4. The authentication method according to claim 1, wherein: in the step (1), the extraction is ultrasonic extraction; the extraction time is 30 min.
5. The authentication method according to claim 1, wherein: in the step (1), the volume-to-mass ratio of the trichloromethane to the drug to be detected is 1ml:1 g.
6. The authentication method according to claim 1, wherein: in the step (2), the sample amount is 10-20 μ l.
7. The authentication method according to claim 1, wherein: in the step (3), the wavelength of the ultraviolet light is 365 nm.
8. The authentication method according to claim 1, wherein: in the step (3), the inspection is performed at a temperature of 4-25 ℃ and a humidity of 32-75%.
9. The authentication method according to claim 1, wherein: in the step (3), the Rf value is 0.143.
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| CN1077383A (en) * | 1993-01-06 | 1993-10-20 | 江西中医学院附属医院 | Preparation method of Chinese medicine |
| CN1332690C (en) * | 2004-08-02 | 2007-08-22 | 四川亚宝光泰药业有限公司 | Technique for preparing Yueju capsule and quality control method |
| CN100388940C (en) * | 2005-11-21 | 2008-05-21 | 贵州益佰制药股份有限公司 | Quality control method of Chinese medicinal preparation for treating child hyperpyrexia |
| CN100533140C (en) * | 2006-03-23 | 2009-08-26 | 江西汇仁药业有限公司 | Checking method for depression relieving and tranquilizing preparation |
| CN101485762A (en) * | 2008-01-16 | 2009-07-22 | 韩勇 | Quality control method of Chinese medicine preparation |
| CN102335260A (en) * | 2010-07-15 | 2012-02-01 | 中国中医科学院中药研究所 | Processing principle-based individualized and characteristic quality evaluation method for Gardenia jasminoides Ellis decoction pieces |
| CN102120015A (en) * | 2010-10-16 | 2011-07-13 | 秦皇岛皇威制药有限公司 | Traditional Chinese medicine for soothing liver and dispersing depressed vital energy and soothing nerves and sedating mind, and preparation method and quality standard thereof |
| US20170260394A1 (en) * | 2014-09-17 | 2017-09-14 | Dsm Ip Assets B.V. | A new process for producing gardenia blue pigment |
| CN106324174A (en) * | 2015-06-18 | 2017-01-11 | 天津市药品检验所 | Quality standard for traditional Chinese medicine formula granules |
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