Characteristic chromatogram of xian'gan zhiluan oral liquid and construction method and application thereof

Abstract

The application discloses a characteristic map of Xiaan Zhisun oral liquid and a construction method and application thereof, and belongs to the technical field of traditional Chinese medicine detection. The technical problems to be solved are: constructing a characteristic map of Xiaan Zhisun oral liquid with good separation effect, high stability, good repeatability and qualified precision. The technical solution points are: a construction method of a characteristic map of Xiaan Zhisun oral liquid, which comprises the following steps: canceling Zhisun oral liquid, adding methanol, filtering, and obtaining a test sample solution; respectively taking glycyrrhizin, ammonium glycyrrhizinate, haraeanoside, quercitrin, hesperidin and naringin, adding methanol, and preparing control sample solutions; performing HPLC detection analysis on the test sample solution and the control sample solutions to obtain an HPLC characteristic map of Xiaan Zhisun oral liquid; and the mobile phase A of the HPLC detection analysis is acetonitrile, and the mobile phase B is a phosphoric acid aqueous solution.

Description

Technical Field

[0001] This invention provides a characteristic spectrum of an anti-snoring oral liquid, its construction method, and its application, belonging to the field of traditional Chinese medicine detection technology. Background Technology

[0002] Xiaogan Zhihan Oral Liquid is composed of eight herbs: Platycodon grandiflorus, Houttuynia cordata, Perilla frutescens stem, Gleditsia sinensis thorn, Scrophularia ningpoensis, Glycyrrhiza uralensis, Citrus reticulata peel, and Astragalus membranaceus. It is derived from a formula developed through years of clinical experience and is used to treat adenoid hypertrophy in children. The formula's theoretical framework is based on the ascending and descending of Qi, regulating Qi and blood. Platycodon grandiflorus disperses lung Qi, clearing blockages and promoting lung Qi circulation; Gleditsia sinensis thorn promotes detoxification, disperses nodules, and reduces swelling; these are the principal herbs. Citrus reticulata peel and Perilla frutescens stem descend turbid Yin and stop stomach upset; Scrophularia ningpoensis clears lung metal and generates water; Houttuynia cordata clears heat and detoxifies; these are the assistant herbs. Astragalus membranaceus strengthens the Wei Qi, consolidates the exterior, promotes detoxification and tissue regeneration, assists the principal herbs in opening and clearing lung blockages, descending rebellious lung Qi, opening the nasal and pharyngeal orifices, and penetrating both the exterior and interior; this is the guiding herb. Glycyrrhiza uralensis tonifies the lungs and spleen, protects the middle Jiao, and harmonizes the other herbs. The combined effects of these herbs resolve phlegm, clear heat, cool the blood, and disperse nodules.

[0003] The main process for preparing Xiaogan Zhihan oral liquid is as follows: weigh out each medicinal material according to the Xiaogan Zhihan oral liquid formula, add an appropriate amount of water for reflux extraction, concentrate the extract, centrifuge, concentrate again to obtain an extract, and then mix the extract with an appropriate amount of pharmaceutical excipients to make an oral liquid or syrup.

[0004] The core efficacy of traditional Chinese medicine compound formulas lies in the synergistic effect of multiple herbs, components, and targets. The stability of their intrinsic quality directly relates to clinical efficacy and medication safety. However, current research on Xiaogan Zhihan oral liquid lacks quality standards, making it difficult to meet the "holistic control" requirements of compound preparations. Thin-layer chromatography (TLC) is an important experimental technique for the rapid separation and qualitative analysis of small amounts of substances. The equipment and operation are relatively simple, and the sample volume and time required are minimal. However, existing TLC methods mainly focus on single-herb analysis, and there are currently no reports on TLC identification analysis methods for the entire Xiaogan Zhihan oral liquid formula. The common practice is to identify each herb individually based on its corresponding TLC identification conditions. This is insufficient to meet the efficiency requirements of TLC identification in actual production. Furthermore, the complex composition of Xiaogan Zhihan oral liquid means that single-herb TLC analysis methods cannot accurately eliminate interference. Therefore, there is an urgent need to develop a TLC identification method for Xiaogan Zhihan oral liquid.

[0005] Relevant patent documents retrieved: This document discloses a method for establishing the fingerprint spectrum and the fingerprint spectrum of a traditional Chinese medicine preparation called Jiuwei Buxue Oral Liquid (CN115201389A, published on October 27, 2023). The chromatographic conditions for fingerprinting include: mobile phase A is acetonitrile, and mobile phase B is formic acid solution; gradient elution is used; a reference solution, a test solution, and a negative sample solution are prepared; these solutions are injected into a high-performance liquid chromatograph (HPLC) under the specified chromatographic conditions to obtain the fingerprint spectrum. This study utilizes HPLC... ELSD established a characteristic spectrum detection method for Jiuwei Buxue Oral Liquid, identifying 25 characteristic peaks and identifying 9 characteristic components, including ginsenosides Rg1, Re, Rb1, Rd, astragaloside A, glycyrrhizin, naringin, hesperidin, and nobiletin.

[0006] Relevant non-patent literature retrieved: The journal or book title is *Chinese Journal of Experimental Traditional Medical Formulae*, and the document title is "Simultaneous Determination of Five Components (Glycyrrhizin, Naringin, Hesperidin, Neohesperidin, and Ammonium Glycyrrhizate) in Jianpi Shuwei Gel by HPLC," Volume 2, Issue 2, 2015, Publication Date 2015. This document discloses: the establishment of an HPLC method for the simultaneous determination of five components (glycyrrhizin, naringin, hesperidin, neohesperidin, and ammonium glycyrrhizate) in Jianpi Shuwei Gel. The method uses an Agilent ZORBAX Eclipse SB-C18 column (4.6 mm × 150 mm, 5 μm), with a mobile phase of acetonitrile-0.05% phosphoric acid-water gradient elution at a flow rate of 1.0 mL·min⁻¹. The detection wavelengths are 237 nm (glycyrrhizin and ammonium glycyrrhizate) and 283 nm (naringin, hesperidin, and neohesperidin), suitable for the quality control of Jianpi Shuwei Gel.

[0007] The prior art represented by the aforementioned literature has at least the following unresolved technical problems or defects: Currently, although naringin, hesperidin, glycyrrhizin, and ammonium glycyrrhizate are used to establish characteristic profiles, there is a lack of a quality control method for anti-snoring oral liquid. Summary of the Invention

[0008] The purpose of this invention is to provide: A characteristic spectrum of an anti-snoring oral liquid, its construction method and application, and related technologies are disclosed to solve technical problems such as constructing a characteristic spectrum of an anti-snoring oral liquid with good separation effect, high stability, good repeatability and qualified precision, or a combination thereof.

[0009] Terminology Explanation: Unless otherwise defined, all technical terms used herein have the same meanings as commonly understood by one of ordinary skill in the art to which the subject matter pertains. Unless otherwise stated, all patents, patent inventions, and publications cited throughout this document are incorporated herein by reference in their entirety. Where multiple definitions exist for terms, the definitions provided in this chapter shall prevail.

[0010] It should be understood that the above brief description and the following detailed description are exemplary and for illustrative purposes only, and do not limit the subject matter of the invention in any way. In this invention, the singular is used in conjunction with the plural unless otherwise specifically stated. It should also be noted that, unless otherwise stated, the use of “or” or “or” means “and / or”. Furthermore, the use of the term “comprising” and other forms such as “including,” “containing,” and “contains” are not limiting.

[0011] Definitions of standard chemical terms can be found in the reference "Chinese Pharmacopoeia (2025 Edition)".

[0012] Unless otherwise specified, conventional methods within the scope of the art, such as HPLC detection methods, shall be used.

[0013] Unless specifically defined herein, the use of all commercially available products herein employs standard techniques. For example, it may be carried out using the manufacturer's instructions for use with the kit, or in accordance with methods known in the art or the description of this invention. The techniques and methods described herein can generally be implemented according to conventional methods well known in the art, based on the descriptions in the various summary and more specific documents cited and discussed in this specification.

[0014] The terms “optional / arbitrary” or “optionally / arbitrarily” mean that the event or situation described below may or may not occur, including both the occurrence and non-occurrence of the event or situation.

[0015] In a first aspect, the present invention provides: a method for constructing a feature map of an anti-snoring oral liquid, comprising the following steps: S1: Remove the anti-snoring oral solution, add methanol, filter, and the test solution is obtained; S2: Take glycyrrhizin, glycyrrhizic acid ammonium, harpagoside, quercetin, hesperidin, and naringin respectively, add methanol, and prepare reference solutions; S3: Perform HPLC analysis on the test solution and the reference solution to obtain the HPLC characteristic chromatogram of Xiaogan Zhihan Oral Liquid; The mobile phase A used in the HPLC analysis was acetonitrile, and the mobile phase B was an aqueous solution of phosphoric acid.

[0016] The oral liquid for eliminating glandular snoring includes: Platycodon grandiflorus, Houttuynia cordata, Perilla frutescens stem, Gleditsia sinensis thorn, Scrophularia ningpoensis, Glycyrrhiza uralensis, Citrus reticulata peel, and Astragalus membranaceus.

[0017] The concentration of glycyrrhizin in step S2 is 0.09-0.15 mg / mL.

[0018] The preferred concentration of glycyrrhizin in step S2 is 0.09 mg / mL, 0.10 mg / mL, 0.11 mg / mL, 0.12 mg / mL, 0.13 mg / mL, 0.14 mg / mL, 0.15 mg / mL, or any combination thereof.

[0019] The concentration of ammonium glycyrrhizate in step S2 is 0.09-0.15 mg / mL.

[0020] The concentration of ammonium glycyrrhizate in step S2 is preferably 0.09 mg / mL, 0.10 mg / mL, 0.11 mg / mL, 0.12 mg / mL, 0.13 mg / mL, 0.14 mg / mL, 0.15 mg / mL, or any combination thereof.

[0021] The concentration of harpagoside in step S2 is 0.09-0.15 mg / mL.

[0022] The preferred concentration of harpagoside in step S2 is 0.09 mg / mL, 0.10 mg / mL, 0.11 mg / mL, 0.12 mg / mL, 0.13 mg / mL, 0.14 mg / mL, 0.15 mg / mL, or any combination thereof.

[0023] The concentration of quercetin in step S2 is 0.09-0.15 mg / mL.

[0024] The preferred concentration of quercetin in step S2 is 0.09 mg / mL, 0.10 mg / mL, 0.11 mg / mL, 0.12 mg / mL, 0.13 mg / mL, 0.14 mg / mL, 0.15 mg / mL, or any combination thereof.

[0025] The concentration of hesperidin in step S2 is 0.09-0.15 mg / mL.

[0026] The preferred concentration of hesperidin in step S2 is 0.09 mg / mL, 0.10 mg / mL, 0.11 mg / mL, 0.12 mg / mL, 0.13 mg / mL, 0.14 mg / mL, 0.15 mg / mL, or any combination thereof.

[0027] In step S2, the concentration of naringin in naringin is 0.09-0.15 mg / mL.

[0028] The preferred concentration of naringin in step S2 is 0.09 mg / mL, 0.10 mg / mL, 0.11 mg / mL, 0.12 mg / mL, 0.13 mg / mL, 0.14 mg / mL, 0.15 mg / mL, or any combination thereof.

[0029] The chromatographic column used for HPLC detection and analysis is a C18 column.

[0030] The HPLC detection wavelength is 205-210 nm, the flow rate is 1-1.5 mL / min, the column temperature is 29-31 °C, and the injection volume is 5-10 μL.

[0031] The gradient elution conditions for HPLC detection and analysis are as follows: 0-10 min, mobile phase A volume fraction 19%; 10-30 min, mobile phase A volume fraction 19%→25%; 30-39 min, mobile phase A volume fraction 25%→32%; 39-40 min, mobile phase A volume fraction 32%→45%; 40-50 min, mobile phase A volume fraction 45%→80%; 50-55 min, mobile phase A volume fraction 80%→19%; 55-60 min, mobile phase A volume fraction 19%.

[0032] The volume fraction of the phosphoric acid aqueous solution is 0.05-0.15%.

[0033] Based on further solutions to the technical problems of the present invention, or simultaneous solutions to multiple technical problems, the preferred solution in the technical solution provided in the first aspect of the present invention includes: Flow rate optimization, column temperature optimization, and elution method optimization.

[0034] This technical solution, having solved the technical problem of "constructing a characteristic spectrum of anti-snoring oral liquid", further solves the technical problem of "constructing a characteristic spectrum of anti-snoring oral liquid with good separation effect, high stability, good repeatability and qualified precision".

[0035] Secondly, the present invention provides: a characteristic spectrum of an anti-snoring oral liquid containing 6 common peaks; The six common peaks are: peak 1 is glycyrrhizin, peak 2 is naringin, peak 3 is quercetin, peak S is hesperidin, peak 5 is harpagoside, and peak 6 is ammonium glycyrrhizate. With peak S as the reference peak, the relative retention times of the six common peaks are as follows: peak 1 is 0.5-0.6 min, peak 2 is 0.7-0.8 min, peak 3 is 0.85-0.95 min, peak S is 1.00 min, peak 5 is 1.8-2.3 min, and peak 6 is 2.5-3.5 min.

[0036] Preferably, the relative retention times of the six common peaks are as follows: peak 1 is 0.54 min, peak 2 is 0.74 min, peak 3 is 0.90 min, peak 4 is 1.00 min, peak 5 is 2.03 min, and peak 6 is 2.74 min.

[0037] Thirdly, the present invention provides the application of the above-described method and / or the above-described characteristic spectrum of the anti-snoring oral liquid in the quality detection and quality control of the anti-snoring oral liquid.

[0038] The present invention has at least the following beneficial effects: Compared with existing technologies, the present invention has better technical effects in constructing a characteristic spectrum of anti-snoring oral liquid with good separation effect, high stability, good repeatability and qualified precision.

[0039] According to experimental tests, in the stability test of this invention, the relative peak area RSD of each chromatographic peak was 0.11%~1.68%; in the repeatability test of this invention, the relative peak area RSD of each chromatographic peak was 0.09%~1.31%; and in the precision test of this invention, the relative peak area RSD of each chromatographic peak was 0.18%~1.50%.

[0040] According to experimental tests, the feature spectrum of the anti-snoring oral liquid of the present invention has better separation.

[0041] Furthermore, based on the present invention: Based on the comparison of Example 1 and Comparative Examples 1-3, this invention employs a combination of specific elution procedures and other technical means to achieve new technical effects, constructing a characteristic spectrum of the anti-snoring oral liquid with good separation effect, high stability, good repeatability, and qualified precision. The combined technical effect is superior to the sum of the effects of each individual technical means. Attached Figure Description

[0042] Figure 1 The characteristic chromatograms are those of the anti-snoring oral liquid and various control solutions of Example 1.

[0043] Figure 2 This is the HPLC chromatogram of Comparative Example 1.

[0044] Figure 3 This is the HPLC chromatogram of Comparative Example 2.

[0045] Figure 4 This is the HPLC chromatogram of Comparative Example 3.

[0046] Figure 5 The image shows the HPLC chromatogram of Example 5, where S1-S9 are arranged from top to bottom.

[0047] Figure 6 HPLC chromatogram for detection at a wavelength of 200 nm.

[0048] Figure 7 HPLC chromatogram for detection at a wavelength of 254 nm.

[0049] Figure 8 HPLC chromatogram for detection at a wavelength of 300 nm.

[0050] Figure 9 HPLC chromatogram at a flow rate of 0.6 mL / min Figure 10 HPLC chromatogram at a flow rate of 0.8 mL / min Figure 11 The HPLC chromatogram is obtained at a flow rate of 1.0 mL / min. Peak 1 is glycyrrhizin, peak 2 is naringin, peak 3 is quercetin, peak S is hesperidin, peak 5 is harpagoside, and peak 6 is ammonium glycyrrhizate.

[0051] in, Figure 1 , Figure 5-11 The horizontal axis represents the retention time, and the vertical axis represents the response value. Whether the axis is clear or not does not affect the technical effect of the present invention. Detailed Implementation

[0052] The following non-limiting embodiments are intended to enable those skilled in the art to gain a more comprehensive understanding of the present invention, but do not limit the invention in any way. The following content is merely an exemplary description of the scope of protection claimed by the present invention, and those skilled in the art can make various changes and modifications to the present invention based on the disclosed content, and such changes should also fall within the scope of protection claimed by the present invention.

[0053] The present invention will be further described below by way of specific embodiments. Unless otherwise specified, all instruments, devices, equipment, reagents, products, etc., used in the embodiments of the present invention are obtained through conventional commercial means.

[0054] The anti-snoring oral liquid used in this embodiment of the invention is prepared according to the preparation method of Example 5 of CN122005685A.

[0055] Example 1: Method for establishing the HPLC characteristic chromatogram of an anti-snoring oral liquid. Includes the following steps: (1) Preparation of the test solution Accurately weigh 1g of the anti-snoring oral solution (Suzhou Wusongjiang Pharmaceutical Co., Ltd., 241001), add 50ml of 80% methanol, seal tightly, sonicate (600W power, 40KHZ frequency) for 30 minutes, filter, and collect the filtrate.

[0056] (2) Preparation of reference solution Accurately weigh appropriate amounts of each reference standard, dissolve them in methanol, and prepare reference standard solutions with the following concentrations: glycyrrhizin 0.121 mg / mL, ammonium glycyrrhizate 0.109 mg / mL, harpagoside 0.111 mg / mL, quercetin 0.103 mg / mL, hesperidin 0.102 mg / mL, and naringin 0.104 mg / mL. Shake each reference standard solution well before use.

[0057] (3) Perform HPLC detection on the above-obtained test and reference solutions. HPLC detection was performed using a C18 column with dimensions of 4.6 mm × 250 mm and a diameter of 5 μm.

[0058] The HPLC detection conditions were as follows: mobile phase A was acetonitrile, and mobile phase B was a 0.1% (v / v) aqueous solution of phosphoric acid. The detection wavelength was 210 nm, the flow rate was 1 mL / min, the column temperature was 30 °C, and the injection volume was 10 μL. The gradient elution conditions were as follows: 0-10 min, mobile phase A volume fraction 19%; 10-30 min, mobile phase A volume fraction 19%→25%; 30-39 min, mobile phase A volume fraction 25%→32%; 39-40 min, mobile phase A volume fraction 32%→45%; 40-50 min, mobile phase A volume fraction 45%→80%; 50-55 min, mobile phase A volume fraction 80%→19%; 55-60 min, mobile phase A volume fraction 19%.

[0059] See results Figure 1 S1 is a glycyrrhizin reference solution, with peak 1 being glycyrrhizin, a characteristic component of licorice; S2 is a naringin reference solution, with peak 2 being naringin, a characteristic component of dried tangerine peel; S3 is a quercetin reference solution, with peak 3 being quercetin, a characteristic component of houttuynia cordata; S4 is a hesperidin reference solution, with peak S being hesperidin, a characteristic component of dried tangerine peel; S5 is a harpagoside reference solution, with peak 5 being harpagoside, a characteristic component of scrophularia ningpoensis; and S6 is an ammonium glycyrrhizate reference solution, with peak 6 being ammonium glycyrrhizate, a characteristic component of licorice.

[0060] S7 is an oral solution for eliminating glandular snoring. It has peaks at peaks 1, 2, 3, S, 5, and 6. Peak S has a larger peak area and is more stable, so it is designated as the reference peak.

[0061] Methodological Validation of Fingerprinting (4) Stability test The test solution was analyzed at 0, 6, 10, 18 and 24 h according to the HPLC detection method described above. The results showed that the relative retention time RSD of each chromatographic peak was 0.01%~1.09% and the relative peak area RSD of each chromatographic peak was 0.11%~1.68%, which met the technical requirements of characteristic chromatograms.

[0062] (5) Repeatability test Take 6 samples from the same batch, prepare test solutions according to the method in the example, and then determine them according to the HPLC detection method to examine the relative retention time and relative peak area (RSD) of each common peak.

[0063] The results showed that the relative retention time (RSD) of each chromatographic peak was 0.01%–0.65%, and the relative peak area (RSD) of each chromatographic peak was 0.09%–1.31%, which met the technical requirements of characteristic chromatograms.

[0064] (6) Precision test The test solution obtained in the example was injected six times consecutively according to the HPLC detection method, and the relative retention time and relative peak area RSD of each common peak were examined. The results showed that the RSD of the relative retention time of each chromatographic peak was 0.05%~0.99%, and the RSD of the relative peak area of ​​each chromatographic peak was 0.18%~1.50%, which met the technical requirements of characteristic chromatograms.

[0065] (7) Parameter determination Example 2: Investigation of Detection Wavelength Through comparative analysis of liquid chromatography spectra, this invention found that the peaks at 200, 254, and 300 nm were relatively few. Figure 6 , Figure 7 , Figure 8 The peak height and peak area ratios among the chromatographic peaks are also uneven, which cannot fully reflect the components of the preparation. At 210 nm, there are more peaks in the spectrum, and the fingerprint peaks of each component are well separated. Taking into account the number of chromatographic peaks, baseline and signal response strength, 210 nm was determined to be the optimal detection wavelength for the characteristic spectrum.

[0066] Example 3: Investigation of Flow Rate This invention selected three different flow rates—0.6 mL / min, 0.8 mL / min, and 1.0 mL / min—for determination. The chromatograms are shown below. Figure 9 , Figure 10 , Figure 11 It was found that the chromatographic peaks of each component were well separated at a flow rate of 1.0 mL / min, so 1.0 mL / min was determined to be the optimal detection flow rate for the characteristic chromatogram.

[0067] Example 4: Investigation of column temperature Column temperature is one of the important parameters in high-performance liquid chromatography (HPLC). Changes in column temperature can lead to peak retention time shifts, affecting the separation of components and the similarity comparison of characteristic chromatograms. This invention compared different column temperatures of 25℃, 30℃, and 35℃. Under the same other chromatographic conditions, the separation effect of each peak was best at 30℃; therefore, the column temperature was determined to be 30℃.

[0068] Example 5 Sample Detection The method described in Example 1 was used to test three batches of samples, and the results are as follows: Figure 5 .

[0069] S1 is glycyrrhizin reference solution, S2 is naringin reference solution, S3 is quercetin reference solution, S4 is hesperidin reference solution, S5 is harpagoside reference solution, and S6 is ammonium glycyrrhizate reference solution.

[0070] S7 (Suzhou Wusongjiang Pharmaceutical Co., Ltd., 241001), S8 (Suzhou Wusongjiang Pharmaceutical Co., Ltd., 241002), and S9 (Suzhou Wusongjiang Pharmaceutical Co., Ltd., 241003) are different batches of Xiaogan Zhihan Oral Liquid. All of them have clear peaks at peaks 1, 2, 3, S, 5, and 6, indicating that this fingerprinting method can reliably detect multiple medicinal characteristics such as glycyrrhizin, naringin, quercetin, hesperidin, harpagoside, and ammonium glycyrrhizate in the product. The method has good reproducibility and can meet the quality control requirements of Xiaogan Zhihan Oral Liquid.

[0071] Comparative Example 1 The difference from Example 1 is as follows: The gradient elution program was modified using acetonitrile (mobile phase A) - 0.1% phosphoric acid aqueous solution (mobile phase B). The gradient elution conditions were as follows: From 0 to 20 min, the volume fraction of mobile phase A is 15%; from 20 to 30 min, the volume fraction of mobile phase A changes from 15% to 18%; from 30 to 50 min, the volume fraction of mobile phase A changes from 18% to 33%; from 50 to 65 min, the volume fraction of mobile phase A changes from 33% to 60%; and from 65 to 70 min, the volume fraction of mobile phase A is 60%.

[0072] See results Figure 2 As can be seen from the chromatogram, the peak separation is poor when using this elution program.

[0073] Comparative Example 2 The difference from Example 1 is as follows: The gradient elution program was modified using acetonitrile (mobile phase A) - water (mobile phase B). The gradient elution conditions are as follows: 0-10 min, the volume fraction of mobile phase A is 5%; 10-15 min, the volume fraction of mobile phase A changes from 5% to 18%; 15-20 min, the volume fraction of mobile phase A changes from 18% to 33%; 20-45 min, the volume fraction of mobile phase A changes from 33% to 70%; 45-60 min, the volume fraction of mobile phase A is 70%.

[0074] See results Figure 3 Using this elution program resulted in poor peak shape and poor chromatographic peak resolution.

[0075] Comparative Example 3 The difference from Example 1 is as follows: The mobile phase was changed to acetonitrile (mobile phase A) - 0.2% phosphoric acid aqueous solution (mobile phase B), with all other conditions remaining unchanged.

[0076] As a result, Figure 4 Using this mobile phase, the chromatographic peaks could not be separated, and the peak shapes did not meet the standards.

[0077] Finally, it should be noted that the above content is only used to illustrate the technical solution of the present invention, and is not intended to limit the scope of protection of the present invention. Simple modifications or equivalent substitutions made by those skilled in the art to the technical solution of the present invention do not depart from the essence and scope of the technical solution of the present invention.

Claims

1. A method for constructing a characteristic spectrum of an oral liquid for eliminating glandular secretions and relieving snoring, characterized in that, Includes the following steps: S1: Remove the anti-snoring oral solution, add methanol, filter, and the test solution is obtained; S2: Take glycyrrhizin, glycyrrhizic acid ammonium, harpagoside, quercetin, hesperidin, and naringin respectively, add methanol, and prepare reference solutions; S3: Perform HPLC analysis on the test solution and the reference solution to obtain the HPLC characteristic chromatogram of Xiaogan Zhihan Oral Liquid; The mobile phase A used in the HPLC analysis was acetonitrile, and the mobile phase B was an aqueous solution of phosphoric acid.

2. The construction method according to claim 1, characterized in that, The ingredients of the oral liquid for eliminating glandular snoring include: Platycodon grandiflorus, Houttuynia cordata, Perilla frutescens stem, Gleditsia sinensis thorn, Scrophularia ningpoensis, Glycyrrhiza uralensis, Citrus reticulata peel, and Astragalus membranaceus.

3. The construction method according to claim 1, characterized in that, In step S2, the concentrations of glycyrrhizin, ammonium glycyrrhizate, harpagoside, quercetin, hesperidin, and naringin are 0.09-0.15 mg / mL, 0.09-0.15 mg / mL, 0.09-0.15 mg / mL, 0.09-0.15 mg / mL, and 0.09-0.15 mg / mL.

4. The construction method according to claim 1, characterized in that, The chromatographic column used for HPLC detection and analysis is a C18 column.

5. The construction method according to claim 1, characterized in that, The HPLC detection wavelength is 205-210 nm, the flow rate is 1-1.5 mL / min, the column temperature is 29-31 °C, and the injection volume is 5-10 μL.

6. The construction method according to claim 1, characterized in that, The gradient elution conditions for HPLC detection and analysis were as follows: 0-10 min, mobile phase A volume fraction 19%; 10-30 min, mobile phase A volume fraction 19%→25%; 30-39 min, mobile phase A volume fraction 25%→32%; 39-40 min, mobile phase A volume fraction 32%→45%; 40-50 min, mobile phase A volume fraction 45%→80%; 50-55 min, mobile phase A volume fraction 80%→19%; 55-60 min, mobile phase A volume fraction 19%.

7. The construction method according to claim 1, characterized in that, The volume fraction of the phosphoric acid aqueous solution is 0.05-0.15%.

8. The characteristic spectrum of the anti-snoring oral liquid constructed by the method according to any one of claims 1-7, characterized in that, It contains 6 common peaks; The six common peaks are: peak 1 is glycyrrhizin, peak 2 is naringin, peak 3 is quercetin, peak S is hesperidin, peak 5 is harpagoside, and peak 6 is ammonium glycyrrhizate. With peak S as the reference peak, the relative retention times of the six common peaks are as follows: peak 1 is 0.5-0.6 min, peak 2 is 0.7-0.8 min, peak 3 is 0.85-0.95 min, peak S is 1.00 min, peak 5 is 1.8-2.3 min, and peak 6 is 2.5-3.5 min.

9. The feature map according to claim 8, characterized in that, The relative retention times of the six common peaks are as follows: peak 1 is 0.54 min, peak 2 is 0.74 min, peak 3 is 0.90 min, peak S is 1.00 min, peak 5 is 2.03 min, and peak 6 is 2.74 min.

10. The application of the method according to any one of claims 1-7 and / or the characteristic spectrum of the anti-snoring oral liquid according to any one of claims 8-9 in the quality testing and quality control of the anti-snoring oral liquid.

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