Characteristic spectrum of flaxseed decoction pieces and preparations thereof, construction method and application thereof

Abstract

The present invention belongs to the field of identification of traditional Chinese medicine, and specifically provides a characteristic spectrum of flax seed slices and preparations thereof, and a construction method and application thereof, wherein the construction method comprises the following steps: (1) mixing the flax seed slice preparation with an alcohol solution, ultrasonically filtering to obtain a first test solution; (2) mixing the flax seed slices with water, boiling, filtering, drying the filtrate, and then mixing with the alcohol solution, ultrasonically filtering to obtain a second test solution; (3) performing UPLC detection on the first test solution and the second test solution respectively, and selecting peaks with consistent retention time, good peak shape and high separation degree as characteristic peaks according to the detection results, selecting S peaks with determined components and good peak shape from the characteristic peaks, calculating the relative retention time of other characteristic peaks relative to the S peak, and obtaining a characteristic spectrum. The constructed characteristic spectrum provided by the present invention has good repeatability, high precision and good stability, and can effectively identify the quality of flax seed medicines.

Description

Technical Field

[0001] The invention belongs to the field of traditional Chinese medicine identification, and specifically relates to a characteristic spectrum of flaxseed slices and preparations thereof, a construction method and application thereof, and especially relates to a characteristic spectrum of flaxseed slices and preparations thereof with high precision, a construction method and application thereof. Background Art

[0002] Flaxseed is the dried mature seed of the flax plant Linum usitatissimum L. of the linaceae family. It is sweet in taste and neutral in nature. It belongs to the lung, liver and large intestine meridians. It has the effects of moistening dryness and relieving constipation, nourishing blood and dispelling wind. It is used for constipation caused by dry intestines, dry skin, itching and hair loss. Studies have shown that the chemical components in flaxseed mainly contain lignans, polyphenols, flavonoids, unsaturated fatty acids, sugars, cyclic peptides and amino acid compounds. To ensure the clinical efficacy of flaxseed, it is necessary to conduct overall quality control of its active ingredients. Flaxseed standard decoction freeze-dried powder is a traditional Chinese medicine product obtained by extracting, concentrating, separating and drying flaxseed slices through modern pharmaceutical technology. At the same time, it is particularly important to control the quality of its products using modern detection technology. Among them, the flaxseed characteristic spectrum method established by high-performance liquid chromatography can not only perform multi-component qualitative analysis of flaxseed slices and flaxseed preparations, control the quality of flaxseed, ensure the consistency of the material basis, but also quantitatively determine the tryptophan component in flaxseed, thereby achieving the stability and effectiveness of the entire process.

[0003] At present, in the qualitative and quantitative research on flaxseed in the 2020 edition of the Chinese Pharmacopoeia, there are only physical and chemical identification and gas phase detection items for fatty oils, and there is no high-performance liquid chromatography method for quality control of its non-oil component content and characteristic spectrum. CN114076806A discloses a fingerprint spectrum detection method for linseed oil and its application, wherein the detection method uses fingerprint spectrum for detection, including the following steps: using gas chromatography-mass spectrometry to construct a phytosterol reference fingerprint spectrum of different varieties of linseed oil; the detection conditions of the gas chromatography include: chromatographic column: 5% phenyl-95% methyl polysiloxane column; split ratio: 38-43:1; heating program: initial temperature 160-200℃, maintain 0.5-2min, heat to 280-320℃ at 1-8℃ / min, and maintain 20-30min. The invented method can be used to distinguish and identify different varieties of linseed oil, and can achieve rapid and effective identification of linseed oil, which is of certain significance for linseed oil quality control and adulteration identification. However, the method uses gas chromatography-mass spectrometry detection, which has high detection costs, is difficult to industrialize and popularize, and the fingerprint only contains plant sterol components, and does not involve other components at all.

[0004] Since there is no method for simultaneously controlling the quality of flaxseed slices and flaxseed slice preparations, how to provide a characteristic spectrum of flaxseed slices and flaxseed slice preparations and effectively control the quality of flaxseed slices and flaxseed slice preparations has become an urgent problem to be solved. Summary of the invention

[0005] In view of the shortcomings of the prior art, the purpose of the present invention is to provide a characteristic spectrum of flaxseed slices and preparations thereof, and a method for constructing and using the same, and in particular to provide a characteristic spectrum of flaxseed slices and preparations thereof with high precision, and a method for constructing and using the same. The characteristic spectrum constructed by the present invention has good repeatability, high precision, and good stability, and can effectively identify the quality of flaxseed medicines.

[0006] In order to achieve the purpose of the invention, the present invention adopts the following technical solutions:

[0007] In a first aspect, the present invention provides a method for constructing a characteristic spectrum of flaxseed slices and preparations thereof, the construction method comprising the following steps:

[0008] (1) mixing the linseed decoction preparation and the alcohol solution with ultrasound, and filtering to obtain a first test solution;

[0009] (2) mixing the flaxseed slices with water and boiling them, filtering and drying the filtrate, and then mixing with an alcohol solution by ultrasonication and filtering to obtain a second test solution;

[0010] (3) The first test solution and the second test solution were subjected to UPLC detection respectively. According to the detection results, the peaks with consistent retention time, good peak shape and high separation were selected as characteristic peaks, and the peaks with definite components and good peak shape were selected as S peaks among the characteristic peaks. The relative retention times of other characteristic peaks relative to S peak were calculated, and the characteristic spectrum of flaxseed decoction pieces and their preparations was obtained.

[0011] There is no order distinction between steps (1) and (2).

[0012] The above method constructs a characteristic spectrum together with flax seed pieces and flax seed pieces preparations, and the obtained characteristic spectrum can not only identify the flax seed pieces, but also identify the flax seed pieces preparations; and the characteristic spectrum obtained by UPLC detection of the first test sample solution and the second test sample solution by a specific method has good repeatability, high precision and good durability.

[0013] The flaxseed decoction preparation includes flaxseed standard decoction freeze-dried powder, flaxseed formula granules and the like.

[0014] Preferably, the solid-liquid ratio of the flaxseed decoction preparation to the alcohol solution in step (1) is 1:(90-110) g / mL.

[0015] Preferably, the ultrasonication time in step (1) is 25-35 min.

[0016] Preferably, the solid-liquid ratio of the flaxseed slices to water in step (2) is 1:(90-110) g / mL.

[0017] Preferably, the decocting temperature in step (2) is 95-100° C. and the decocting time is 25-35 min.

[0018] Preferably, the solid-liquid ratio of the flaxseed slices to the alcohol solution in step (2) is 1:(18-22) g / mL.

[0019] Preferably, the ultrasonication time in step (2) is 25-35 min.

[0020] Preferably, the alcohol solution is a methanol-water solution, and the volume fraction of the methanol-water solution is 65-75%.

[0021] Wherein, the solid-liquid ratio of the linseed slice preparation to the alcohol solution can be 1:90 g / mL, 1:95 g / mL, 1:100 g / mL, 1:105 g / mL or 1:110 g / mL, etc., the ultrasonic time in step (1) can be 25 min, 26 min, 27 min, 28 min, 29 min, 30 min, 31 min, 32 min, 33 min, 34 min or 35 min, etc., the solid-liquid ratio of the linseed slice preparation to water can be 1:90 g / mL, 1:95 g / mL, 1:100 g / mL, 1:105 g / mL or 1:110 g / mL, etc., the decoction temperature in step (2) can be 95° C., 96° C., 97° C., 98° C., 99° C. or 100° C., etc., and the decoction time can be 25 min, 26 min, 27 min, 28 min, 29 min, 30 min, 31 min, 32 min, 33 min, 34 min or 35 min, etc. The solid-liquid ratio of the linseed slices to the alcohol solution can be 1:18 g / mL, 1:19 g / mL, 1:20 g / mL, 1:21 g / mL or 1:22 g / mL, the ultrasonic time in step (2) can be 25 min, 26 min, 27 min, 28 min, 29 min, 30 min, 31 min, 32 min, 33 min, 34 min or 35 min, and the volume fraction of the methanol aqueous solution can be 65%, 66%, 67%, 68%, 69%, 70%, 71%, 72%, 73%, 74% or 75%, but are not limited to the above-listed values. Other values ​​not listed within the above numerical range are also applicable.

[0022] The present invention can fully extract the effective components in the flaxseed decoction piece preparation and the flaxseed decoction piece by controlling the above parameters, thereby improving the accuracy of subsequent detection and characteristic spectrum.

[0023] Preferably, the filler of the chromatographic column for UPLC detection in step (3) is octadecylsilane bonded silica gel.

[0024] Preferably, the mobile phase for UPLC detection in step (3) comprises mobile phase A and mobile phase B, wherein mobile phase A is acetonitrile, and mobile phase B is aqueous phosphoric acid solution, and the mass fraction of the aqueous phosphoric acid solution is 0.08-0.12%.

[0025] Preferably, the flow rate of the UPLC detection in step (3) is 0.28-0.32 mL / min, and the column temperature is 32-38°C.

[0026] Preferably, the wavelength of the UPLC detection in step (3) is 210-220 nm, preferably 217 nm.

[0027] Wherein, the mass fraction of the aqueous phosphoric acid solution can be 0.08%, 0.09%, 0.1%, 0.11% or 0.12%, etc., the flow rate can be 0.28 mL / min, 0.29 mL / min, 0.3 mL / min, 0.31 mL / min or 0.32 mL / min, etc., the column temperature can be 32° C., 33° C., 34° C., 35° C., 36° C., 37° C. or 38° C., etc., and the wavelength can be 210 nm, 211 nm, 212 nm, 213 nm, 214 nm, 215 nm, 216 nm, 217 nm, 218 nm, 219 nm or 220 nm, etc., but are not limited to the values ​​listed above, and other values ​​not listed within the above numerical range are equally applicable.

[0028] Preferably, the elution procedure of the UPLC detection in step (3) is as follows:

[0029] From 0 to 8 minutes, the volume fraction of mobile phase A changes from 2% to 5% at a constant rate, and the volume fraction of mobile phase B changes from 98% to 95% at a constant rate;

[0030] From 8 to 15 minutes, the volume fraction of mobile phase A changes from 5% to 12% at a constant rate, and the volume fraction of mobile phase B changes from 95% to 88% at a constant rate;

[0031] From 15 to 21 minutes, the volume fraction of mobile phase A changes from 12% to 14% at a constant rate, and the volume fraction of mobile phase B changes from 88% to 86% at a constant rate;

[0032] During the 21st to 35th minute, the volume fraction of mobile phase A changed from 14% to 18% at a constant rate, and the volume fraction of mobile phase B changed from 86% to 82% at a constant rate.

[0033] The above-mentioned specific elution procedure can effectively distinguish the components in the sample, with high peak separation and obvious peaks, and can obtain characteristic peaks with better peak shapes, thereby improving the accuracy of detection and characteristic spectra, and can also significantly shorten the elution time and improve detection efficiency.

[0034] In a second aspect, the present invention provides a characteristic spectrum of flaxseed slices and preparations thereof obtained by the construction method as described above, wherein the characteristic spectrum has 7 characteristic peaks, which are arranged in ascending order of retention time, with peak 1 being the S peak, and the relative retention times of peaks 2, 3, 4, 5, 6 and 7 being 1.59±10%, 1.71±10%, 1.92±10%, 2.00±10%, 3.14±10% and 4.27±10%, respectively.

[0035] The peak component No. 1 is tryptophan.

[0036] In a third aspect, the present invention provides the use of the characteristic spectrum of the flaxseed pieces and preparations thereof as described above in the quality judgment of flaxseed medicines.

[0037] In a fourth aspect, the present invention further provides a method for determining the quality of a flaxseed drug, comprising: detecting different batches of flaxseed drugs using the UPLC detection method described above, performing median processing on the detection results, and obtaining a standard characteristic spectrum in combination with the characteristic spectrum described above; detecting a sample to be tested using the UPLC detection method described above, determining characteristic peaks based on the characteristic spectrum described above, and then performing similarity judgment or relative retention time judgment to determine whether the sample to be tested is a qualified product or a failed product.

[0038] In the similarity judgment, the similarity between the characteristic peak of the sample to be tested and the characteristic peak in the standard characteristic spectrum is calculated; when the similarity is not less than 0.85, the sample to be tested is qualified, and when the similarity is less than 0.85, the sample to be tested is unqualified.

[0039] In the relative retention time judgment, the relative retention time of each characteristic peak of the sample to be tested is calculated and compared with the relative retention time of each characteristic peak in the characteristic spectrum as described above. If the relative retention time of the characteristic peak of the sample to be tested falls outside the relative retention time range of the characteristic peak in the characteristic spectrum as described above, the sample to be tested is unqualified; if the relative retention time of all characteristic peaks of the sample to be tested falls within the relative retention time range of the characteristic peak in the characteristic spectrum as described above, the sample to be tested is qualified.

[0040] The flaxseed medicine is flaxseed decoction pieces or flaxseed decoction piece preparations.

[0041] The above method uses the prepared characteristic spectrum to detect the sample to be tested, which can effectively distinguish whether the sample to be tested is qualified, and provides a new method for quality judgment of flaxseed medicines.

[0042] Compared with the prior art, the present invention has the following beneficial effects:

[0043] The invention provides a method for constructing a characteristic spectrum of flaxseed pieces and a preparation thereof. The characteristic spectrum is constructed by constructing a characteristic spectrum of the flaxseed pieces and the flaxseed pieces preparation together, so that the obtained characteristic spectrum can identify the flaxseed pieces and the flaxseed pieces preparation, and the overall quality control of the flaxseed can be performed. The characteristic spectrum obtained by performing UPLC detection on a first test sample solution and a second test sample solution by a specific method has good repeatability, high precision and good durability. The components in the sample can be effectively distinguished through a specific elution procedure, the peak separation is high, the peaks are obvious, characteristic peaks with good peak shapes can be obtained, the accuracy of detection and characteristic spectrum can be improved, the elution time can be significantly shortened, the detection efficiency can be improved, the method is simple and fast, and it is convenient for industrial application, and the detection cost can be reduced. BRIEF DESCRIPTION OF THE DRAWINGS

[0044] Figure 1 is the characteristic spectrum of Example 1;

[0045] Figure 2 It is the characteristic spectrum of comparative example 1;

[0046] Figure 3 It is the characteristic spectrum of comparative example 2;

[0047] Figure 4 It is the characteristic spectrum of comparative example 3;

[0048] Figure 5 This is a liquid phase result diagram of the test of freeze-dried powder of flaxseed standard decoction.

[0049] Figure 6 This is a diagram of the liquid phase results of the flaxseed herbal medicine testing test. DETAILED DESCRIPTION

[0050] The technical solution of the present invention is further described below by specific implementation methods. It should be understood by those skilled in the art that the embodiments are only to help understand the present invention and should not be regarded as specific limitations of the present invention.

[0051] The instruments and reagents used in the following examples are as follows:

[0052] Instruments: Waters UPLC H-Class ultra-high performance liquid chromatograph; electronic analytical balance (XP26, ME104E, Mettler Toledo; BSA124S, Sartorius; JY20002, Shanghai Sunny Hengping Scientific Instrument Co., Ltd.); KQ-500DB ultrasonic cleaning machine (Kunshan Ultrasonic Electronic Equipment Factory);

[0053] Reagents: acetonitrile (Fisher Chemical) and phosphoric acid (Fisher Scientific) were of chromatographic grade, methanol was of analytical grade, and water was purified water from Watsons.

[0054] Example 1

[0055] This embodiment provides a characteristic spectrum of flaxseed slices and preparations thereof, and the specific construction method is as follows:

[0056] Take an appropriate amount of lyophilized powder of standard flaxseed decoction, grind it into powder, accurately weigh 0.1g, put it into a stoppered conical flask, accurately add 10mL of 70% methanol aqueous solution, stopper it tightly, weigh it, and treat it with ultrasound (power 250W, frequency 40kHz) for 30min, take it out, let it cool, weigh it again, make up the lost weight with 70% methanol aqueous solution, shake it well, filter it, and take the filtrate to obtain the first test solution;

[0057] Take an appropriate amount of flaxseed slices, grind them into powder, accurately weigh 0.5g, add 50mL of water, boil for 30 minutes, filter, evaporate the filtrate, accurately add 10mL of 70% methanol aqueous solution, plug it tightly, weigh it, ultrasonically treat it (power 250W, frequency 40kHz) for 30min, take it out, cool it, weigh it again, make up the lost weight with 70% methanol aqueous solution, shake it well, filter it, and take the filtrate to obtain the second test solution;

[0058] Accurately pipette 1 μL of the first test solution and the second test solution respectively, and inject into high performance liquid chromatography for determination.

[0059] The chromatographic conditions are as follows: a chromatographic column with octadecylsilane bonded silica as filler (column length 100 mm, inner diameter 2.1 mm, particle size 1.7 μm), acetonitrile as mobile phase A, 0.1% phosphoric acid solution as mobile phase B, gradient elution as specified in the table below; detection wavelength 217 nm; column temperature 35° C.; flow rate 0.3 mL per minute.

[0060]

[0061] The results are made into feature maps, such as Figure 1 shown.

[0062] according to Figure 1The results showed that 7 peaks with consistent retention time, high separation, good peak shape and peak time covering the entire elution process were selected as characteristic peaks, which were recorded as peaks 1-7 respectively. Peak 1 (identified as tryptophan peak) was taken as the S peak, and the relative retention times of other peaks were calculated. The results were as follows: 1.59 (peak 2), 1.71 (peak 3), 1.92 (peak 4), 2.00 (peak 5), 3.14 (peak 6), and 4.27 (peak 7), and the characteristic spectrum was obtained.

[0063] Comparative Example 1

[0064] This comparative example provides a characteristic spectrum of flaxseed slices and preparations thereof, and the construction method is consistent with Example 1 except that the chromatographic conditions are as follows.

[0065] The chromatographic conditions are as follows: a chromatographic column with octadecylsilane bonded silica as filler (column length 250 mm, inner diameter 4.6 mm, particle size 5 μm), acetonitrile as mobile phase A, 0.1% phosphoric acid solution as mobile phase B, gradient elution as specified in the table below; detection wavelength 260 nm; column temperature 35° C.; flow rate 1 mL per minute.

[0066]

[0067] The results are as follows Figure 2 shown.

[0068] Comparative Example 2

[0069] This comparative example provides a characteristic spectrum of flaxseed slices and preparations thereof, and the construction method is consistent with Example 1 except that the chromatographic conditions are as follows.

[0070] The chromatographic conditions are as follows: a chromatographic column with octadecylsilane bonded silica as filler (column length 100 mm, inner diameter 2.1 mm, particle size 1.8 μm), acetonitrile as mobile phase A, 0.1% phosphoric acid solution as mobile phase B, gradient elution as specified in the table below; detection wavelength 220 nm; column temperature 35° C.; flow rate 0.4 mL per minute.

[0071]

[0072] The results are as follows Figure 3 shown.

[0073] Comparative Example 3

[0074] This comparative example provides a characteristic spectrum of flaxseed slices and preparations thereof, and the construction method is consistent with Example 1 except that the elution procedure is as follows.

[0075]

[0076] The results are as follows Figure 4 shown.

[0077] From the above results, it can be found that the present invention can achieve high chromatographic peak separation by controlling the gradient elution program, can effectively obtain characteristic peaks, and improve the accuracy of detection and characteristic spectra; while the peak position of the spectrum of comparative example 1 is quite different from that of embodiment 1, the baseline is uneven, and a large number of peaks overlap; in comparative example 2, a large number of peaks overlap at around 20 minutes; in comparative example 3, the baseline is also unequal at around 20-33 minutes, resulting in the inability to confirm the characteristic peaks.

[0078] Repeatability test:

[0079] Take 6 portions of lyophilized powder of flaxseed standard decoction, and measure according to the method provided in Example 1, and calculate the relative retention time of each characteristic peak. The results are as follows:

[0080]

[0081] It can be found that the relative retention time RSD of each characteristic peak is in the range of 0.8-1.0%, indicating that the repeatability of the characteristic spectrum is good.

[0082] Intermediate precision test:

[0083] Six portions of lyophilized powder of standard flaxseed decoction were taken and measured according to the method provided in Example 1 (the ultra-high performance liquid chromatograph was replaced with another Waters UPLC H-Class, TUV detector), and the relative retention time of each characteristic peak was calculated. The results are as follows:

[0084]

[0085] In the characteristic spectrum obtained by Waters UPLC H-Class, TUV detector, the relative retention time RSD of each characteristic peak is in the range of 0.6-1.3%, and the relative retention time RSD range between different instruments is 0.9-1.9%, indicating that the relative peak area of ​​the characteristic spectrum between different instruments meets the analysis requirements.

[0086] Stability test:

[0087] The test solution was prepared according to the method of Example 1, and the test was performed according to the method of Example 1 at 0, 2, 4, 6, 8, 12, and 24 hours after preparation, and the relative retention time of each characteristic peak was calculated. The results are as follows:

[0088]

[0089] The above results show that the characteristic spectrum obtained by the construction method provided by the present invention has good stability, the chemical components in the solution are stable within 24 hours, and the relative retention time RSD of each characteristic peak is in the range of 1.5-1.9%.

[0090] Accuracy test:

[0091] Take an appropriate amount of tryptophan reference substance, accurately weigh it, and add 70% methanol aqueous solution to make a solution containing 253μg per 1mL. Take 9 portions of linseed standard decoction freeze-dried powder (KL190730-741600-01, tryptophan content is 9.85mg / g) in three parallel groups, 0.05g per portion, accurately weigh it, and accurately add 1mL of tryptophan reference substance solution (0.252547mg tryptophan) and 9mL of 70% methanol aqueous solution, 2mL of tryptophan reference substance solution (0.505094mg tryptophan) and 8mL of 70% methanol aqueous solution, 3mL of tryptophan reference substance solution (0.757642mg tryptophan) and 7mL of 70% methanol aqueous solution in a ratio of 1:0.5, 1:1, and 1:1.5, respectively, and then detect according to the liquid phase conditions in Example 1. The recovery rate is calculated according to the following formula, and the results are as follows:

[0092]

[0093]

[0094]

[0095] The measured recovery rate ranged from 95.6% to 101.8%, with an average recovery rate of 99.1% and an RSD value of 2.2%, which met the recovery rate requirements of the methodology validation, indicating that the characteristic spectrum obtained using this construction method has high accuracy.

[0096] Accurately weigh an appropriate amount of tryptophan reference substance, place it in a 50-mL volumetric flask, add methanol to make a solution containing 0.5123 mg per 1 mL, and obtain the tryptophan reference substance mother solution as linear 1; accurately pipette 1 mL of the tryptophan reference substance mother solution of linear 1, place it in a 2-mL volumetric flask, and add methanol to the scale as linear 2; accurately pipette 1 mL of the tryptophan reference substance mother solution of linear 1, place it in a 5-mL volumetric flask, and add methanol to the scale as linear 3; accurately pipette 1 mL of the tryptophan reference substance mother solution of linear 1, place it in a 10-mL volumetric flask, and add methanol to the scale as linear 4; accurately pipette 1 mL of the tryptophan reference substance mother solution of linear 1, place it in a 20-mL volumetric flask, and add methanol to the scale as linear 5; accurately pipette 1 mL of the tryptophan reference substance mother solution of linear 1, place it in a 50-mL volumetric flask, and add methanol to the scale as linear 6. Accurately pipette 1 μL of the above filtrate and inject it into a high performance liquid chromatograph. Determine the peak area of ​​the tryptophan chromatographic peak according to the method of Example 1. Draw a standard curve with the peak area of ​​the tryptophan chromatographic peak as the ordinate and the concentration of tryptophan as the abscissa. The regression equation of tryptophan is y=3099742.83x-18347.44, R 2=0.999, and its linear range is 0.0102-0.5123 mg / mL. The linear equation is used to investigate the parameters in the construction method of the present invention.

[0097] The lyophilized powder of standard decoction of flaxseed was taken and tested according to the method in Example 1, and the column temperature, flow rate, chromatographic column (the stationary phase was replaced with Waters ACQUITY HSS T3 (2.1mm×100mm, 1.8μm), WatersCORTECS T3 (2.1mm×100mm, 1.6μm) and Waters ACQUITY BEH Shield RP18 (2.1 mm × 100 mm, 1.7 μm)) and the mass fraction of phosphoric acid aqueous solution were changed to investigate the durability of the construction method. The results are as follows:

[0098]

[0099]

[0100]

[0101]

[0102] It can be found that the method provided by the present invention has good durability for different column temperatures, flow rates, chromatographic columns and phosphoric acid mass fractions, and the RSD value does not exceed 0.86%.

[0103] Flaxseed standard decoction freeze-dried powder test:

[0104] 15 batches of linseed standard decoction freeze-dried powder were taken and tested according to the method in Example 1. The test spectrum was fitted to obtain a standard characteristic spectrum, and the characteristic peaks were determined according to the characteristic spectrum obtained in Example 1, and the similarity was calculated. The results are shown in the following table and Figure 5 As shown:

[0105]

[0106] The similarities between the characteristic spectra of 15 batches of linseed standard decoction freeze-dried powder and the control characteristic spectra were 0.982-0.999, all higher than 0.85, and all were qualified products.

[0107] Flaxseed decoction test:

[0108] 15 batches of flaxseed slices were taken and tested according to the method in Example 1. The test spectrum was fitted to obtain a standard characteristic spectrum. The characteristic peaks were determined according to the characteristic spectrum obtained in Example 1, and the similarity was calculated. The results are shown in the following table and Figure 6 As shown:

[0109]

[0110]

[0111] The similarity between the characteristic spectra of 15 batches of flaxseed pieces and the control characteristic spectra was 0.933-0.996, all higher than 0.85, and all were qualified products.

[0112] The above detection experiments fully prove that the characteristic spectrum and the construction method thereof provided by the present invention can effectively judge the quality of flaxseed medicines, and provide a new method for judging the quality of flaxseed medicines.

[0113] The applicant declares that the present invention uses the above-mentioned embodiments to illustrate the characteristic spectrum of the flaxseed drink and its preparation, its construction method and application, but the present invention is not limited to the above-mentioned embodiments, that is, it does not mean that the present invention must rely on the above-mentioned embodiments to be implemented. Those skilled in the art should understand that any improvement of the present invention, equivalent replacement of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.

[0114] The preferred embodiments of the present invention are described in detail above. However, the present invention is not limited to the specific details in the above embodiments. Within the technical concept of the present invention, a variety of simple modifications can be made to the technical solution of the present invention, and these simple modifications all belong to the protection scope of the present invention.

[0115] It should also be noted that the various specific technical features described in the above specific embodiments can be combined in any suitable manner without contradiction. In order to avoid unnecessary repetition, the present invention will not further describe various possible combinations.

Claims

1. A method for constructing a characteristic spectrum of linseed slices and preparations thereof, characterized in that: The construction method comprises the following steps: (1) mixing the linseed decoction preparation and the alcohol solution by ultrasonication, and filtering to obtain a first test solution; (2) Mixing the flaxseed slices with water and boiling them, filtering and drying the filtrate, and then mixing with an alcohol solution and ultrasonicating the mixture, and filtering the mixture to obtain a second test solution; (3) The first test solution and the second test solution are subjected to UPLC detection respectively. According to the detection results, the peaks with consistent retention time, good peak shape and high separation are selected as characteristic peaks, and the peaks with certain components and good peak shape are selected as S peaks among the characteristic peaks. The relative retention times of other characteristic peaks relative to S peak are calculated, and the characteristic spectrum of flaxseed decoction pieces and their preparations is obtained; The alcohol solution is a methanol-water solution, and the volume fraction of the methanol-water solution is 65-75%; The filler of the chromatographic column for UPLC detection in step (3) is octadecylsilane bonded silica gel; Step (3) The mobile phase for UPLC detection includes mobile phase A and mobile phase B, wherein mobile phase A is acetonitrile, and mobile phase B is a phosphoric acid aqueous solution, and the mass fraction of the phosphoric acid aqueous solution is 0.08-0.12%; The elution procedure of the UPLC detection in step (3) is as follows: From 0 to 8 minutes, the volume fraction of mobile phase A changes from 2% to 5% at a constant rate, and the volume fraction of mobile phase B changes from 98% to 95% at a constant rate; From 8 to 15 minutes, the volume fraction of mobile phase A changed from 5% to 12% at a constant rate, and the volume fraction of mobile phase B changed from 95% to 88% at a constant rate; From 15 to 21 minutes, the volume fraction of mobile phase A changed from 12% to 14% at a constant rate, and the volume fraction of mobile phase B changed from 88% to 86% at a constant rate; From 21 to 35 minutes, the volume fraction of mobile phase A changed from 14% to 18% at a constant rate, and the volume fraction of mobile phase B changed from 86% to 82% at a constant rate; There is no order in which steps (1) and (2) are performed.

2. The construction method according to claim 1, characterized in that: The solid-liquid ratio of the linseed decoction preparation to the alcohol solution in step (1) is 1:(90-110) g / mL.

3. The construction method according to claim 1, characterized in that: The ultrasonic treatment time in step (1) is 25-35 minutes.

4. The construction method according to claim 1, characterized in that: The solid-liquid ratio of the flaxseed slices to water in step (2) is 1:(90-110) g / mL.

5. The construction method according to claim 1, characterized in that: The decoction temperature in step (2) is 95-100° C. and the decoction time is 25-35 min.

6. The construction method according to claim 1, characterized in that: In step (2), the solid-liquid ratio of the linseed slices to the alcohol solution is 1:(18-22) g / mL.

7. The construction method according to claim 1, characterized in that: The ultrasonic treatment time in step (2) is 25-35 minutes.

8. The construction method according to claim 1, characterized in that: The flow rate of the UPLC detection in step (3) is 0.28-0.32 mL / min, and the column temperature is 32-38°C.

9. The construction method according to claim 1, characterized in that: The wavelength of the UPLC detection in step (3) is 210-220 nm.

10. The construction method according to claim 9, characterized in that: The wavelength of the UPLC detection in step (3) is 217 nm.

11. A method for judging the quality of flaxseed medicine, characterized in that: Different batches of flaxseed medicines are tested by the UPLC detection method in the method for constructing the characteristic spectrum of the flaxseed slices and preparations thereof according to any one of claims 1 to 10, the test results are median processed, and a standard characteristic spectrum is obtained in combination with the characteristic spectrum; the sample to be tested is tested by the UPLC detection method in the method for constructing the characteristic spectrum of the flaxseed slices and preparations thereof according to any one of claims 1 to 10, characteristic peaks are determined according to the characteristic spectrum, and then similarity judgment or relative retention time judgment is performed to determine whether the sample to be tested is a qualified product or a failed product; In the similarity judgment, the similarity between the characteristic peak of the sample to be tested and the characteristic peak in the standard characteristic spectrum is calculated; when the similarity is not less than 0.85, the sample to be tested is qualified, and when the similarity is less than 0.85, the sample to be tested is unqualified; In the relative retention time judgment, the relative retention time of each characteristic peak of the sample to be tested is calculated and compared with the relative retention time of each characteristic peak in the characteristic spectrum. If the relative retention time of the characteristic peak of the sample to be tested falls outside the relative retention time range of the characteristic peak in the characteristic spectrum, the sample to be tested is unqualified; if the relative retention time of all characteristic peaks of the sample to be tested falls within the relative retention time range of the characteristic peak in the characteristic spectrum, the sample to be tested is qualified; The flaxseed medicine is flaxseed decoction pieces or flaxseed decoction piece preparations.

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