Quality detection method and detection device for safflower Xiaoyao tablets
Through the thin-layer chromatography identification method of key components in Honghua Xiaoyao tablets, the problems of complexity of existing detection methods and waste of resources are solved, and faster, economical and accurate detection results are achieved.
Patent Information
- Application Number
- CN202411575665.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-06
- Publication Date
- 2025-02-14
AI Technical Summary
The current quality detection method of Honghua Xiaoyao tablets has problems such as complex pre-processing and weak specificity, which leads to a lot of time consumption, large organic reagent consumption, and serious waste of resources, which affects the detection efficiency and accuracy.
A quality detection method including identification method of angelica, mint, licorice, white peony, and bamboo leaf Bupleurum in safflower Xiaoyao tablets is adopted. This method uses silicone G thin-layer plate and specific developer to determine whether the components are qualified.
The detection process is simplified, the consumption of samples and organic solvents is reduced, the rapidity, economicality and accuracy of detection is improved, and the detection effect is significantly improved.
Smart Images
Figure CN119438192A_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of quality detection of traditional Chinese medicine preparations, and in particular relates to a quality detection method and a detection device for Honghua Xiaoyao tablets. Background Art
[0002] Honghua Xiaoyao Tablets is a Chinese patent medicine, mainly used to treat liver qi discomfort, chest and flank pain, dizziness, loss of appetite, menstrual disorders, breast pain or facial chloasma. Its main ingredients include angelica, white peony, atractylodes, tuckahoe, safflower, Gleditsia sinensis, Bupleurum chinense, mint, licorice, etc. It has the effects of soothing the liver, regulating qi and promoting blood circulation. In order to test its quality, it is necessary to apply the detection method.
[0003] The quality inspection standards of the current quality inspection methods have the disadvantages of complex pre-treatment and low specificity, which consumes more time and organic reagents, resulting in a waste of resources and affecting the inspection efficiency and accuracy of this product. In order to solve the above problems, a quality inspection method and inspection device for Honghua Xiaoyao tablets are urgently needed. Summary of the invention
[0004] The purpose of the present invention is to propose a quality inspection method and inspection device for Honghua Xiaoyao Tablets in order to solve the problems that the quality inspection standards of the current quality inspection methods have the disadvantages of complex pre-treatment and low specificity, thereby consuming more time and organic reagents, resulting in waste of resources and affecting the inspection efficiency and accuracy of the product.
[0005] In order to achieve the above object, the present invention adopts the following technical scheme: a quality detection method of Honghua Xiaoyao Tablets, including identification of angelica and mint in Honghua Xiaoyao Tablets, the steps are as follows:
[0006] A1. Prepare Honghua Xiaoyao Tablets test solution, Angelica sinensis reference medicinal material solution, and menthol reference substance solution;
[0007] A2. Take the Honghua Xiaoyao Tablets test solution, Angelica sinensis reference medicinal material solution, and Menthol reference substance solution prepared in A1, and spot them on the same silica gel G thin layer plate respectively. Use a mixture of n-hexane and ethyl acetate as the developing agent for development. Then dry and inspect after color development. Based on the inspection results, determine whether the Angelica sinensis and mint components in Honghua Xiaoyao Tablets are qualified.
[0008] As a further description of the above technical solution:
[0009] In A1 and A2, the identification method of angelica and mint is that the spots developed under the conditions of temperature 10-30°C and humidity 18-88% are rich in color and have clear outlines. In A2, the volume ratio of n-hexane to ethyl acetate in the developing solvent is 8:2.
[0010] As a further description of the above technical solution:
[0011] In A1, the preparation of the test solution includes: grinding Honghua Xiaoyao tablets, adding ether for ultrasonic treatment, filtering, setting aside the residue, concentrating the filtrate to 1 ml, and preparing the test solution. The preparation of the Angelica sinensis control medicinal material solution includes: taking Angelica sinensis control medicinal materials, and preparing a control medicinal material solution according to the preparation method of the test solution. The preparation of the menthol reference substance solution includes: taking a menthol reference substance, adding ether to dissolve it to prepare a 2 mg / ml solution, which is the menthol reference substance solution.
[0012] A quality detection method for Honghua Xiaoyao tablets, further comprising identifying licorice and white peony root in Honghua Xiaoyao tablets, the steps being as follows:
[0013] B1. Prepare Honghua Xiaoyao Tablets test solution, Licorice reference drug solution, and Paeoniflorin reference solution;
[0014] B2. Take the Honghua Xiaoyao Tablets test solution, licorice reference medicinal material solution and paeoniflorin reference solution prepared in step B1, respectively spot them on the same silica gel G thin layer plate, develop them with a mixture of ethyl acetate, formic acid, glacial acetic acid and water as the developing agent, then dry and inspect after color development, and judge whether the licorice and white peony ingredients in Honghua Xiaoyao Tablets are qualified based on the inspection results.
[0015] As a further description of the above technical solution:
[0016] In B1 and B2, the identification method of licorice and white peony root is that the spots developed under the conditions of temperature 10-30°C and humidity 18-88% are rich in color and have clear outlines. In B2, the volume ratio of ethyl acetate, formic acid, glacial acetic acid and water in the developing agent is 15:1:1:2.
[0017] As a further description of the above technical solution:
[0018] In B1, the preparation of the test solution includes: taking the above-mentioned reserved drug residue, adding methanol for ultrasonic treatment, filtering and evaporating the filtrate to dryness, dissolving the residue in water and extracting by shaking with water-saturated n-butanol, washing the n-butanol layer with ammonia test solution, evaporating the n-butanol solution to dryness, and dissolving the residue in methanol to obtain the test solution.
[0019] As a further description of the above technical solution:
[0020] In B1, the preparation of the licorice control medicinal material solution includes: taking licorice control medicinal material and preparing a control medicinal material solution according to the above-mentioned test solution preparation method, and the preparation of the paeoniflorin reference solution includes: taking a paeoniflorin reference, adding methanol to dissolve it to prepare a 1 mg / ml solution, which is the paeoniflorin reference solution.
[0021] A quality detection method for Honghua Xiaoyao tablets also includes identifying Bupleurum chinense in Honghua Xiaoyao tablets, and the steps are as follows:
[0022] C1. Prepare Honghua Xiaoyao Tablets test solution and Bamboo Leaf Bupleurum control medicinal material solution;
[0023] C2. Take the test sample solution and the reference medicinal material solution of bamboo leaf bupleurum prepared in step C1, respectively spot them on the same silica gel G thin layer plate, develop them with a mixture of ethyl acetate, methanol and water as the developing agent, then dry and inspect them after color development, and judge whether the bamboo leaf bupleurum component in Honghua Xiaoyao tablets is qualified based on the inspection results.
[0024] As a further description of the above technical solution:
[0025] In C1 and C2, the identification method of Bupleurum chinense is that the spots developed under the conditions of temperature 10-30° C. and humidity 18-88% are rich in color and have clear outlines. In C2, the volume ratio of ethyl acetate, methanol and water in the developing agent is 16:3:2.
[0026] As a further description of the above technical solution:
[0027] In the C1, the test solution is the Honghua Xiaoyao Tablets test solution prepared in C1. In the C1, the preparation of the reference medicinal material solution of Bamboo Leaf Bupleurum includes: taking Bamboo Leaf Bupleurum reference medicinal material, decocting it with water, filtering it, extracting the filtrate by shaking it with ether, and discarding the ether solution.
[0028] The present invention also discloses a quality inspection device for Honghua Xiaoyao tablets, comprising a casing, an expansion chamber is arranged inside the casing, a slide groove is arranged inside the expansion chamber, an oscillation table is fixed below the expansion chamber, a controller is fixedly installed on an outer wall of one side of the casing, a machine door is installed on the front side of the casing, an observation window is inlaid on the outside of the machine door, a liquid filling port and a thin layer plate insertion port are arranged on the top of the casing, and a liquid discharge port is arranged at the bottom of the casing.
[0029] In summary, due to the adoption of the above technical solution, the beneficial effects of the present invention are:
[0030] In the present invention, the identification method of angelica, mint, white peony root, liquorice and bamboo-leaf bupleurum provided by the method simplifies and integrates the existing technology, reduces the consumption of samples and organic solvents, and is simpler, faster, more economical and reasonable than the existing technology. By comparing and optimizing the method conditions, the bamboo-leaf bupleurum identification method provided by the present invention can obtain spots with clearer contours and more enriched colors, greatly improving the overall quality detection effect and the practical application effect of the overall method. The detection device makes the entire operation process more efficient and safe, which helps to improve experimental efficiency and detection effect and ensure the health and safety of personnel. BRIEF DESCRIPTION OF THE DRAWINGS
[0031] Figure 1 , Figure 2 The present invention is the development result of testing angelica and mint negative samples and different developing agents on silica gel G thin layer plate;
[0032] Figure 3 The main spot identified by the present invention in the test of Angelica sinensis is ligustilide, the main component of volatile oil:
[0033] Figure 4 This is the result of the development of angelica and mint in the low humidity environment in Test Example 1 of the present invention;
[0034] Figure 5 This is the result of the development of angelica and mint in the high humidity environment in Test Example 1 of the present invention;
[0035] Figure 6 This is the result of the development of angelica and mint at 10°C in Test Example 1 of the present invention;
[0036] Figure 7 This is the result of the development of angelica and mint at 20°C in Test Example 1 of the present invention;
[0037] Figure 8 This is the result of the development of angelica and mint at 30°C in Test Example 1 of the present invention;
[0038] Fig. 9 , Fig.10 The results of the present invention on the development of negative samples of licorice and white peony root and different developing agents on silica gel G thin layer plates are as follows:
[0039] Fig.11 The results of developing the test sample solutions of different extraction solvents on the silica gel G thin layer plate for testing the identification method of licorice in the present invention are as follows:
[0040] Fig.12 This is the result of the development of licorice and white peony root in the low humidity environment in Test Example 2 of the present invention;
[0041] Fig.13 This is the result of the development of licorice and white peony root in the high humidity environment in Test Example 2 of the present invention;
[0042] Fig.14 This is the result of the development of Licorice and White Peony Root at 10°C in Test Example 2 of the present invention;
[0043] Fig.15 This is the result of the development of Licorice and White Peony Root at 20°C in Test Example 2 of the present invention;
[0044] Fig.16 The results of the development of licorice and white peony root at 30°C in Experimental Example 2 of the present invention;
[0045] Fig.17 , Fig.18 The present invention is the development result of testing the negative sample of Bupleurum chinense and different developing agents and color development methods on silica gel G thin layer plate;
[0046] Fig.19 This is the result of the expansion of Bupleurum chinense in the low humidity environment in Test Example 3 of the present invention;
[0047] Fig. 20 This is the result of the expansion of Bupleurum chinense in a high humidity environment in Test Example 3 of the present invention;
[0048] Fig.21 This is the result of the expansion of Bupleurum chinense at 10°C in Experimental Example 3 of the present invention;
[0049] Fig. 22 This is the result of the expansion of Bupleurum chinense at 20°C in Experimental Example 3 of the present invention;
[0050] Fig.23 This is the result of the expansion of Bupleurum chinense at 30°C in Experimental Example 3 of the present invention;
[0051] Fig.24 The present invention is a flow chart of a quality inspection method for Honghua Xiaoyao tablets.
[0052] Fig.25 It is a schematic diagram of the three-dimensional structure of a quality inspection device for Honghua Xiaoyao tablets.
[0053] Legend:
[0054] 1. Casing; 2. Development chamber; 3. Oscillation table; 4. Controller; 5. Door; 6. Observation window; 7. Liquid filling port; 8. Thin layer plate insertion port; 9. Liquid discharge port. DETAILED DESCRIPTION
[0055] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0056] The present invention provides a quality detection method for Honghua Xiaoyao tablets, comprising identifying angelica and mint in Honghua Xiaoyao tablets, and the steps are as follows:
[0057] A1. Prepare a test solution of Honghua Xiaoyao Tablets, a reference medicinal material solution of Angelica sinensis, and a reference solution of menthol. The preparation of the test solution comprises: grinding Honghua Xiaoyao Tablets, adding ether for ultrasonic treatment, filtering, reserving the residue for later use, and concentrating the filtrate to 1 ml to prepare a test solution. The preparation of the reference medicinal material solution of Angelica sinensis comprises: taking reference medicinal materials of Angelica sinensis, and preparing a reference medicinal material solution according to the preparation method of the test solution. The preparation of the reference solution of menthol comprises: taking a reference substance of menthol, adding ether to dissolve it to prepare a solution of 2 mg / ml, i.e., the reference solution of menthol;
[0058] A2. Take the Honghua Xiaoyao Tablets test solution, Angelica sinensis reference medicinal material solution, and Menthol reference substance solution prepared in A1, and spot them on the same silica gel G thin layer plate respectively, and develop them with a mixture of n-hexane and ethyl acetate as the developing agent, then dry them, develop the color and inspect them, and judge whether the Angelica sinensis and mint components in the Honghua Xiaoyao Tablets are qualified according to the inspection results. The identification method of Angelica sinensis and mint is that the spots developed under the conditions of temperature 10-30°C and humidity 18-88% are rich in color and clear in outline, and the volume ratio of n-hexane to ethyl acetate in the developing agent is 8:2;
[0059] A quality detection method for Honghua Xiaoyao tablets, further comprising identifying licorice and white peony root in Honghua Xiaoyao tablets, the steps being as follows:
[0060] B1. Prepare a test solution of Honghua Xiaoyao Tablets, a licorice control medicinal material solution, and a peonidin reference substance solution. The preparation of the test solution includes: taking the above-mentioned reserved medicinal residue, adding methanol for ultrasonic treatment, filtering and evaporating the filtrate to dryness, dissolving the residue in water and extracting by shaking with water-saturated n-butanol, washing the n-butanol layer with an ammonia test solution, evaporating the n-butanol solution to dryness, and dissolving the residue in methanol to prepare a test solution. The preparation of the licorice control medicinal material solution includes: taking licorice control medicinal materials and preparing a control medicinal material solution according to the above-mentioned test solution preparation method. The preparation of the peonidin reference substance solution includes: taking a peonidin reference substance and dissolving it in methanol to prepare a 1 mg / ml solution, which is the peonidin reference substance solution;
[0061] B2. Take the Honghua Xiaoyao Tablets test solution, licorice reference medicinal material solution, and paeoniflorin reference substance solution prepared in step B1, and spot them on the same silica gel G thin layer plate respectively, and develop them with a mixed solution of ethyl acetate, formic acid, glacial acetic acid, and water as a developing agent, then dry them, develop the colors, and inspect them, and judge whether the licorice and white peony components in the Honghua Xiaoyao Tablets are qualified according to the inspection results. The identification method of licorice and white peony is that the spots developed under the conditions of temperature 10-30°C and humidity 18-88% are enriched in color and have clear contours, and the volume ratio of ethyl acetate, formic acid, glacial acetic acid, and water in the developing agent is 15:1:1:2;
[0062] A quality detection method for Honghua Xiaoyao tablets also includes identifying Bupleurum chinense in Honghua Xiaoyao tablets, and the steps are as follows:
[0063] C1, preparing a Honghua Xiaoyao Tablets test solution and a Bamboo Leaf Bupleurum control medicinal material solution, wherein the test solution is the Honghua Xiaoyao Tablets test solution prepared in C1, wherein the preparation of the Bamboo Leaf Bupleurum control medicinal material solution in C1 comprises: taking Bamboo Leaf Bupleurum control medicinal material, decocting it with water, filtering it, extracting the filtrate by shaking with ether, and discarding the ether solution;
[0064] C2. Take the test solution and the reference medicinal material solution of bamboo leaf bupleurum prepared in step C1, respectively spot them on the same silica gel G thin layer plate, develop them with a mixture of ethyl acetate, methanol and water as the developing agent, then dry them, develop the colors and inspect them, and judge whether the bamboo leaf bupleurum component in Honghua Xiaoyao tablets is qualified based on the inspection results. The identification method of bamboo leaf bupleurum is that the spots developed under the conditions of temperature 10-30℃ and humidity 18-88% are enriched in color and have clear outlines, and the volume ratio of ethyl acetate, methanol and water in the developing agent is 16:3:2.
[0065] The following are specific embodiments of the above scheme:
[0066] Example 1
[0067] In this embodiment, the angelica and mint in Honghua Xiaoyao tablets were identified as follows:
[0068] Take 15 tablets of this product, remove the film coating, grind finely, add 30ml of ether, ultrasonically treat for 30 minutes, filter, set aside the residue, concentrate the filtrate to 1ml, and use it as the test solution. Take another 0.25g of Angelica sinensis reference medicinal material, and prepare the reference medicinal material solution in the same way. Take menthol reference substance, add ether to prepare a solution containing 2mg per 1ml, and use it as the reference substance solution. According to the thin layer chromatography method (General Rule 0502), take 10-20μl of the above test solution, 2μl of the reference medicinal material solution, and 10μl of the reference substance solution, and spot them on the same silica gel G thin layer plate, use n-hexane-ethyl acetate with a volume ratio of 8:2 as the developing solvent, develop, take out, dry, and examine under ultraviolet light (365nm). Then spray with 5% vanillin sulfuric acid solution and heat at 105℃ until the spots are clearly colored.
[0069] In the chromatogram of the test sample, a fluorescent spot of the same color appears at the corresponding position of the chromatogram of the Angelica sinensis reference medicinal material; a spot of the same color appears at the corresponding position of the chromatogram of the menthol reference substance.
[0070] Example 2
[0071] In this embodiment, the licorice and white peony root in Honghua Xiaoyao tablets were identified as follows:
[0072] Take the drug residue after ether extraction under Example 1, add 40 ml of methanol, ultrasonically treat for 25 minutes, filter, evaporate the filtrate to dryness, add 30 ml of water to the residue to dissolve, shake and extract with 30 ml of water-saturated n-butanol, take the n-butanol solution, wash with 30 ml of ammonia test solution, take the n-butanol solution, evaporate to dryness, and add 2 ml of methanol to the residue to dissolve as the test solution. Take 0.5 g of licorice control medicinal material and prepare the control medicinal material solution in the same way. Take an appropriate amount of paeoniflorin reference substance, add methanol to prepare a solution containing 1 mg per 1 ml as the reference substance solution. According to the thin layer chromatography method (General Rule 0502), 2-5 μl of each of the three solutions mentioned above were respectively spotted on the same silica gel G thin layer plate, and ethyl acetate-formic acid-glacial acetic acid-water with a volume ratio of 15:1:1:2 was used as the developing solvent. The plate was taken out, dried, sprayed with 10% ethanolic sulfuric acid solution, heated at 105°C until the spots were clearly colored, and examined under daylight and ultraviolet light (365nm) respectively.
[0073] In the chromatogram of the test sample, a fluorescent spot of the same color appears at the corresponding position in the chromatogram of the licorice reference medicinal material; a spot of the same color appears at the corresponding position in the chromatogram of the paeoniflorin reference substance.
[0074] Example 3
[0075] In this embodiment, the Radix Bupleuri in Honghua Xiaoyao Tablets was identified as follows:
[0076] Take 1g of the reference medicinal material of Bupleurum chinense, add water and boil for 2 hours, filter, and extract the filtrate with ether twice, 20ml each time, discard the ether solution, and prepare the reference medicinal material solution in the same way as "shake and extract with 30ml of n-butanol saturated with water" in Example 2. Test according to the thin layer chromatography method (General Rule 0502), take 2-5μl of the test solution in Example 2 and the above-mentioned reference medicinal material solution, respectively, and spot them on the same silica gel G thin layer plate, use ethyl acetate-methanol-water with a volume ratio of 16:3:2 as the developing solvent, develop, take out, dry, spray with 4% p-dimethylaminobenzaldehyde 10% sulfuric acid ethanol solution, and blow with hot air until the spots are clearly colored. In the chromatogram of the test sample, spots of the same color appear at the corresponding position of the chromatogram of the reference medicinal material.
[0077] In Examples 1-3, the identification methods for angelica, mint, white peony root, licorice, and bamboo-leaf bupleurum provided simplify and integrate the existing technologies, reduce the consumption of samples and organic solvents, and are simpler, faster, more economical and reasonable than the existing technologies. By comparing and optimizing the method conditions, the bamboo-leaf bupleurum identification method provided by the present invention can obtain spots with clearer contours and more enriched colors, greatly improving the overall quality detection effect and improving the practical application effect of the overall method.
[0078] In addition to Examples 1-3, the following test examples are disclosed:
[0079] Test Example 1
[0080] In this test example, the environmental applicable conditions of the method for identifying angelica and mint in Example 1 were tested, including
[0081] Humidity suitability test
[0082] The experiment investigated the unfolding effects of three different batches of samples at room temperature and different humidity (18% RH and 88% RH);
[0083] Take 10-20 μl of Honghua Xiaoyao Tablets (batch number 8230202, 8230602, 8231101) test solution, 10 μl of angelica-deficient and mint-negative test solution, 2 μl of angelica reference medicinal material solution, and 10 μl of menthol reference solution, and spot them on the same silica gel G plate. Use n-hexane-ethyl acetate with a volume ratio of 8:2 as the developing solvent, develop them in low humidity 18% RH and high humidity 88% RH, take them out, dry them, and examine them under ultraviolet light (365nm). Then spray them with 5% vanillin sulfuric acid solution and heat them at 105°C until the spots are clearly colored.
[0084] Low humidity environment results such as Figure 4 As shown in the figure, number 1 corresponds to menthol reference substance, numbers 2, 3, and 4 correspond to samples with batch numbers 8230202, 8230602, and 8231101 respectively, number 5 corresponds to angelica-deficient and mint-negative samples, and number 6 corresponds to angelica reference medicinal materials.
[0085] High humidity environment results such as Figure 5 As shown in the figure, number 1 corresponds to menthol reference substance, numbers 2, 3, and 4 correspond to samples with batch numbers 8230202, 8230602, and 8231101 respectively, number 5 corresponds to angelica-deficient and mint-negative samples, and number 6 corresponds to angelica reference medicinal materials.
[0086] According to the expansion results, it can be found that the spots corresponding to angelica and mint have clear outlines and rich colors.
[0087] Temperature suitability test
[0088] The experiment investigated the unfolding effects of three different batches of samples at different temperatures (10°C, 20°C, and 30°C) under 45% RH humidity conditions;
[0089] Take 10-20 μl of Honghua Xiaoyao Tablets (batch number 8230202, 8230602, 8231101) test solution, 10-20 μl of angelica-deficient and mint-negative test solution, 2 μl of angelica reference medicinal material solution, and 10 μl of menthol reference solution, and spot them on the same silica gel G plate. Use n-hexane-ethyl acetate with a volume ratio of 8:2 as the developing solvent, develop at 10°C, 20°C, and 30°C, take out, dry, and examine under ultraviolet light (365nm). Then spray with 5% vanillin sulfuric acid solution and heat at 105°C until the spots are clearly colored.
[0090] The results of 10℃ expansion are as follows Figure 6 As shown in the figure, number 1 corresponds to menthol reference substance, numbers 2, 3, and 4 correspond to samples with batch numbers 8230202, 8230602, and 8231101 respectively, number 5 corresponds to angelica-deficient and mint-negative samples, and number 6 corresponds to angelica reference medicinal materials.
[0091] The results of the expansion at 20°C are as follows Figure 7 As shown in the figure, number 1 corresponds to menthol reference substance, numbers 2, 3, and 4 correspond to samples with batch numbers 8230202, 8230602, and 8231101 respectively, number 5 corresponds to angelica-deficient and mint-negative samples, and number 6 corresponds to angelica reference medicinal materials.
[0092] The results of 30℃ expansion are as follows Figure 8 As shown in the figure, number 1 corresponds to menthol reference substance, numbers 2, 3, and 4 correspond to samples with batch numbers 8230202, 8230602, and 8231101 respectively, number 5 corresponds to angelica-deficient and mint-negative samples, and number 6 corresponds to angelica reference medicinal materials.
[0093] According to the expansion results, it can be found that the spots corresponding to angelica and mint have clear outlines and rich colors.
[0094] Test Example 2
[0095] In this test example, the environmental applicable conditions of the method for identifying licorice and white peony root in Example 2 were tested, including
[0096] Humidity suitability test
[0097] The experiment investigated the unfolding effects of three different batches of samples at room temperature and different humidity (18% RH and 88% RH);
[0098] 2-5 μl of each of Honghua Xiaoyao Tablets (batch numbers 8230202, 8230602, and 8231101) test solution, licorice-deficient and white peony-negative test solutions, licorice control medicinal material solution, and paeoniflorin reference solution were taken and spotted on the same silica gel G plate. The plate was developed using ethyl acetate-formic acid-glacial acetic acid-water in a volume ratio of 15:1:1:2. The plate was taken out, dried, sprayed with 10% ethanolic sulfuric acid solution, heated at 105°C until the spots were clearly colored, and examined under daylight and ultraviolet light (365nm), respectively.
[0099] Low humidity environment results such as Fig.12 As shown, number 1 in the figure corresponds to the paeoniflorin reference substance, numbers 2, 3, and 4 correspond to samples with batch numbers 8230202, 8230602, and 8231101, respectively, number 5 corresponds to licorice-deficient and white peony-negative samples, and number 6 corresponds to licorice reference medicinal materials.
[0100] High humidity environment results such as Fig.13 As shown, number 1 in the figure corresponds to the paeoniflorin reference substance, numbers 2, 3, and 4 correspond to samples with batch numbers 8230202, 8230602, and 8231101, respectively, number 5 corresponds to licorice-deficient and white peony-negative samples, and number 6 corresponds to licorice reference medicinal materials.
[0101] According to the expansion results, it can be found that the spots corresponding to licorice and white peony root have clear outlines and rich colors.
[0102] Temperature suitability test
[0103] The experiment investigated the unfolding effects of three different batches of samples at different temperatures (10°C, 20°C, and 30°C) under 45% RH humidity conditions;
[0104] 2-5 μl of each of Honghua Xiaoyao Tablets (batch numbers 8230202, 8230602, and 8231101) test solution, licorice-deficient and white peony-negative test solutions, licorice control medicinal material solution, and paeoniflorin reference solution were taken and spotted on the same silica gel G plate. The plate was developed using ethyl acetate-formic acid-glacial acetic acid-water in a volume ratio of 15:1:1:2. The plate was taken out, dried, sprayed with 10% ethanolic sulfuric acid solution, heated at 105°C until the spots were clearly colored, and examined under daylight and ultraviolet light (365nm), respectively.
[0105] The results of 10℃ expansion are as follows Fig.14 As shown, number 1 in the figure corresponds to the paeoniflorin reference substance, numbers 2, 3, and 4 correspond to samples with batch numbers 8230202, 8230602, and 8231101, respectively, number 5 corresponds to licorice-deficient and white peony-negative samples, and number 6 corresponds to licorice reference medicinal materials.
[0106] The results of the expansion at 20°C are as follows Fig.15As shown, number 1 in the figure corresponds to the paeoniflorin reference substance, numbers 2, 3, and 4 correspond to samples with batch numbers 8230202, 8230602, and 8231101, respectively, number 5 corresponds to licorice-deficient and white peony-negative samples, and number 6 corresponds to licorice reference medicinal materials.
[0107] The results of 30℃ expansion are as follows Fig.16 As shown, number 1 in the figure corresponds to the paeoniflorin reference substance, numbers 2, 3, and 4 correspond to samples with batch numbers 8230202, 8230602, and 8231101, respectively, number 5 corresponds to licorice-deficient and white peony-negative samples, and number 6 corresponds to licorice reference medicinal materials.
[0108] According to the expansion results, it can be found that the spots corresponding to licorice and white peony root have clear outlines and rich colors.
[0109] Test Example 3
[0110] In this test example, the environmental conditions for the method for identifying the root of Radix Bupleuri in Example 3 were tested, including
[0111] Humidity suitability test
[0112] The experiment investigated the unfolding effects of three different batches of samples at room temperature and different humidity (18% RH and 88% RH);
[0113] 2-5 μl of Honghua Xiaoyao Tablets (batch numbers 8230202, 8230602, 8231101) test solution, negative test solution lacking bamboo leaves of Bupleurum chinense, and control medicinal material solution were taken and spotted on the same silica gel G thin layer plate, respectively, and ethyl acetate-methanol-water with a volume ratio of 16:3:2 was used as the developing agent. The plate was developed, taken out, dried, sprayed with 4% p-dimethylaminobenzaldehyde 10% sulfuric acid ethanol solution, and blown with hot air until the spots were clearly colored.
[0114] Low humidity environment results such as Fig.19 As shown in the figure, number 1 corresponds to the paeoniflorin reference substance, numbers 2, 3, and 4 correspond to samples with batch numbers 8230202, 8230602, and 8231101, respectively, and number 5 corresponds to the negative sample lacking Bupleurum chinense.
[0115] High humidity environment results such as Fig. 20 As shown in the figure, number 1 corresponds to the paeoniflorin reference substance, numbers 2, 3, and 4 correspond to samples with batch numbers 8230202, 8230602, and 8231101, respectively, and number 5 corresponds to the negative sample lacking Bupleurum chinense.
[0116] According to the expansion results, it can be found that the spots corresponding to Bupleurum chinense have clear outlines and rich colors.
[0117] Temperature suitability test
[0118] The experiment investigated the unfolding effects of three different batches of samples at different temperatures (10°C, 20°C, and 30°C) under 45% RH humidity conditions;
[0119] 2-5 μl of Honghua Xiaoyao Tablets (batch numbers 8230202, 8230602, 8231101) test solution, Bupleurum chinense negative test solution, and Bupleurum chinense control medicinal material solution were taken and spotted on the same silica gel G plate respectively. Ethyl acetate-methanol-water with a volume ratio of 16:3:2 was used as the developing agent. The plate was developed, taken out, dried, sprayed with 4% p-dimethylaminobenzaldehyde 10% sulfuric acid ethanol solution, and blown with hot air until the spots were clearly colored.
[0120] The results of 10℃ expansion are as follows Fig.21 As shown in the figure, number 1 corresponds to the paeoniflorin reference substance, numbers 2, 3, and 4 correspond to samples with batch numbers 8230202, 8230602, and 8231101, respectively, and number 5 corresponds to the negative sample lacking Bupleurum chinense.
[0121] The results of the expansion at 20°C are as follows Fig. 22 As shown in the figure, number 1 corresponds to the paeoniflorin reference substance, numbers 2, 3, and 4 correspond to samples with batch numbers 8230202, 8230602, and 8231101, respectively, and number 5 corresponds to the negative sample lacking Bupleurum chinense.
[0122] The results of 30℃ expansion are as follows Fig.23 As shown in the figure, number 1 corresponds to the paeoniflorin reference substance, numbers 2, 3, and 4 correspond to samples with batch numbers 8230202, 8230602, and 8231101, respectively, and number 5 corresponds to the negative sample lacking Bupleurum chinense.
[0123] According to the expansion results, it can be found that the spots corresponding to Bupleurum chinense have clear outlines and rich colors.
[0124] Example 4
[0125] The present invention also discloses a quality inspection device for Honghua Xiaoyao tablets, comprising a casing 1, wherein an expansion chamber 2 is arranged inside the casing 1, a slide groove is arranged inside the expansion chamber 2, an oscillation table 3 is fixed below the expansion chamber 2, a controller 4 is fixedly installed on one side outer wall of the casing 1, a machine door 5 is installed on the front side of the casing 1, an observation window 6 is inlaid on the outside of the machine door 5, a liquid filling port 7 and a thin layer plate insertion port 8 are arranged on the top of the casing 1, and a liquid discharge port 9 is arranged at the bottom of the casing 1.
[0126] The above description is only a preferred specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes according to the technical scheme and inventive concept of the present invention within the technical scope disclosed by the present invention, which should be covered by the protection scope of the present invention.
Claims
1. A quality detection method for Honghua Xiaoyao Tablets, characterized in that: Including the identification of angelica and mint in Honghua Xiaoyao tablets, the steps are as follows: A1. Prepare Honghua Xiaoyao Tablets test solution, Angelica sinensis reference medicinal material solution, and menthol reference substance solution; A2. Take the Honghua Xiaoyao Tablets test solution, Angelica sinensis reference medicinal material solution, and Menthol reference substance solution prepared in A1, and spot them on the same silica gel G thin layer plate respectively. Use a mixture of n-hexane and ethyl acetate as the developing agent for development. Then dry and inspect after color development. Based on the inspection results, determine whether the Angelica sinensis and mint components in Honghua Xiaoyao Tablets are qualified.
2. The quality inspection method of Honghua Xiaoyao Tablets according to claim 1, characterized in that: In A1 and A2, the identification method of angelica and mint is that the spots developed under the conditions of temperature 10-30°C and humidity 18-88% are rich in color and have clear outlines. In A2, the volume ratio of n-hexane to ethyl acetate in the developing solvent is 8:
2.
3. The quality detection method of Honghua Xiaoyao Tablets according to claim 2, characterized in that: In A1, the preparation of the test solution includes: grinding Honghua Xiaoyao tablets, adding ether for ultrasonic treatment, filtering, setting aside the residue, concentrating the filtrate to 1 ml, and preparing the test solution. The preparation of the Angelica sinensis control medicinal material solution includes: taking Angelica sinensis control medicinal materials, and preparing a control medicinal material solution according to the preparation method of the test solution. The preparation of the menthol reference substance solution includes: taking a menthol reference substance, adding ether to dissolve it to prepare a 2 mg / ml solution, which is the menthol reference substance solution.
4. The quality inspection method of Honghua Xiaoyao Tablets according to claim 1, characterized in that: It also includes the identification of licorice and white peony root in Honghua Xiaoyao tablets, the steps are as follows: B1. Prepare Honghua Xiaoyao Tablets test solution, Licorice reference drug solution, and Paeoniflorin reference solution; B2. Take the Honghua Xiaoyao Tablets test solution, licorice reference medicinal material solution and paeoniflorin reference solution prepared in step B1, respectively spot them on the same silica gel G thin layer plate, develop them with a mixture of ethyl acetate, formic acid, glacial acetic acid and water as the developing agent, then dry and inspect after color development, and judge whether the licorice and white peony ingredients in Honghua Xiaoyao Tablets are qualified based on the inspection results.
5. The quality detection method of Honghua Xiaoyao Tablets according to claim 4, characterized in that: In B1 and B2, the identification method of licorice and white peony root is that the spots developed under the conditions of temperature 10-30°C and humidity 18-88% are rich in color and have clear outlines. In B2, the volume ratio of ethyl acetate, formic acid, glacial acetic acid and water in the developing agent is 15:1:1:
2.
6. The quality inspection method of Honghua Xiaoyao Tablets according to claim 5, characterized in that: In B1, the preparation of the test solution includes: taking the above-mentioned reserved drug residue, adding methanol for ultrasonic treatment, filtering and evaporating the filtrate to dryness, dissolving the residue in water and extracting by shaking with water-saturated n-butanol, washing the n-butanol layer with ammonia test solution, evaporating the n-butanol solution to dryness, and dissolving the residue in methanol to obtain the test solution.
7. The quality inspection method of Honghua Xiaoyao Tablets according to claim 6, characterized in that: In B1, the preparation of the licorice control medicinal material solution includes: taking licorice control medicinal material and preparing a control medicinal material solution according to the above-mentioned test solution preparation method, and the preparation of the paeoniflorin reference solution includes: taking a paeoniflorin reference, adding methanol to dissolve it to prepare a 1 mg / ml solution, which is the paeoniflorin reference solution.
8. The quality inspection method of Honghua Xiaoyao Tablets according to claim 1, characterized in that: It also includes the identification of Bupleurum chinense in Honghua Xiaoyao Tablets, the steps are as follows: C1. Prepare Honghua Xiaoyao Tablets test solution and Bamboo Leaf Bupleurum control medicinal material solution; C2. Take the test sample solution and the reference medicinal material solution of bamboo leaf bupleurum prepared in step C1, respectively spot them on the same silica gel G thin layer plate, develop them with a mixture of ethyl acetate, methanol and water as the developing agent, then dry and inspect them after color development, and judge whether the bamboo leaf bupleurum component in Honghua Xiaoyao tablets is qualified based on the inspection results.
9. The quality inspection method of Honghua Xiaoyao Tablets according to claim 8, characterized in that: In C1 and C2, the identification method of Bamboo Leaf Bupleurum is that the spots developed under the conditions of temperature 10-30°C and humidity 18-88% are enriched in color and have clear outlines. In C2, the volume ratio of ethyl acetate, methanol and water in the developing agent is 16:3:
2. In C1, the test solution is the Honghua Xiaoyao Tablets test solution prepared in C1. In C1, the preparation of the Bamboo Leaf Bupleurum reference medicinal material solution includes: taking the Bamboo Leaf Bupleurum reference medicinal material, decocting it with water, filtering it, extracting the filtrate by shaking it with ether, and discarding the ether solution.
10. The quality inspection device for Honghua Xiaoyao Tablets according to claim 9, characterized in that: The invention comprises a casing (1), wherein an expansion chamber (2) is arranged inside the casing (1), a slide groove is arranged inside the expansion chamber (2), an oscillation table (3) is fixed below the expansion chamber (2), a controller (4) is fixedly mounted on an outer wall of one side of the casing (1), a machine door (5) is mounted on the front side of the casing (1), an observation window (6) is inlaid on the outside of the machine door (5), a liquid filling port (7) and a thin layer plate insertion port (8) are arranged on the top of the casing (1), and a liquid discharge port (9) is arranged on the bottom of the casing (1).