Method for detecting the mixing uniformity of a mixture containing mirabilite or mirabilite extract

Abstract

The present application relates to the technical field of traditional Chinese medicine detection, in particular to a detection method for the mixing uniformity of a mixture containing mirabilite or mirabilite extract. The detection method comprises the following steps: sampling from the mixture containing mirabilite or mirabilite extract, the sampling points being distributed at different positions of the mixture, each sampling point corresponding to a sample N i ; performing ion chromatography detection on the sample N i respectively, determining the content of Na i in the sample N + ; calculating the relative standard deviation RSD of the content of Na i in each sample N + , and determining whether the mixture containing mirabilite or mirabilite extract is mixed uniformly according to the obtained relative standard deviation RSD. The detection method has high accuracy, high safety factor and high analysis efficiency, can be applied to industrial production, thereby realizing rapid and accurate detection of the mixing uniformity of the mixing process of the mixture containing traditional Chinese medicine preparation, efficient and convenient monitoring of the end point of the mixing time, and providing a new strategy for the quality control of the production process of traditional Chinese medicine preparation containing mirabilite.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of traditional Chinese medicine detection, and particularly relates to a detection method for mixing uniformity of a mixture containing mirabilite or mirabilite extract. BACKGROUND

[0002] Mirabilite is a widely distributed sulfate mineral, which is a crystalline body refined from mirabilite of the mirabilite family of sulfate minerals, mainly containing hydrated sodium sulfate (Na2SO4·10H2O). Mirabilite is cold in nature, bitter and salty in taste, and has the effects of purgation, softening, dampening, clearing heat and reducing swelling, and is often used for treating constipation, dry stool, abdominal pain, intestinal abscess, and other diseases. Modern pharmacological research has found that mirabilite also has the effects of anti-infection, anti-inflammatory, diuresis, and tissue dehydration. Mirabilite is widely used in traditional Chinese medicine preparations due to its good clinical effect, including Dachengqi Decoction, Tiaoweichengqi Decoction, and Taohuochengqi Decoction in Shanghan Lun (Han·Zhang Zhongjing), which are all purgative drugs with the effects of purgation, heat removal, water removal, and accumulation attack. Ancient physicians often used mirabilite in combination with different traditional Chinese medicines to treat diseases such as yangming bowel, chest retention, blood accumulation, intestinal abscess, and erysipelas. For example, in Shanghan Lun, Dachengqi Decoction uses mirabilite (about 45g for three times, stop purgation when the effect is achieved) to soften and dampen, and combines with rhubarb to purge heat and clear the bowels, treating constipation, heat retention, and other diseases of yangming bowel; Daxianxiong Decoction uses mirabilite (about 154g for one dose, stop purgation when the effect is achieved) to purge heat and break retention, and combines with rhubarb and gansuon to remove water and drink, and to clean the intestines and stomach, treating chest retention of water and heat; Taohuochengqi Decoction uses mirabilite (about 27.6g for two doses) to purge heat and soften, and combines with rhubarb and cassia twig to remove heat and purgation without cooling, treating lower jiao blood accumulation of shanghan; in Jin Kui Yaolue, Dahuang Mudan Decoction uses mirabilite (about 45g for three times) to clear heat and purgation, and combines with rhubarb to detoxify and break blood stasis, treating intestinal abscess caused by heat and toxin retention in the intestines; in Tang Bieji Qianjin Yaofang, Shengmajiao uses mirabilite (about 27.6g for two doses) to clear heat and reduce swelling, and combines with shengma to clear heat and detoxify, treating erysipelas and skin swelling.

[0003] The preparation process of the above-mentioned traditional Chinese medicine preparation, mixing is one of the key links. Mixing can refer to the mixing of traditional Chinese medicine extract and auxiliary materials, or the mixing between different traditional Chinese medicine extracts. The uniformity of mixing is the key to ensure the consistency of the internal quality of traditional Chinese medicine preparation. At present, the detection of mixing uniformity of the mixing process of traditional Chinese medicine preparation is mainly through on-line sampling, and the difference in the content of main components is analyzed by off-line detection means, for example: the content of main components at different sampling points is detected by high performance liquid chromatography (HPLC), and the difference in the content of main components is analyzed. This method cannot quickly judge whether the mixing uniformity of the whole batch of mixed materials is qualified due to the complicated sample preparation process, long determination period and low analysis efficiency. In addition, near infrared (NIR) spectroscopy can also be used to detect the mixing uniformity of the mixing process, which has many advantages such as rapidity, non-destructiveness and greenness. However, the accuracy of quantitative analysis of this method depends on the established quantitative model, that is, a certain number of modeling samples are collected, and the near infrared spectrum and chemical analysis value of the samples are measured respectively, and the mathematical relationship between them is established by chemometrics method (becomes a quantitative model). In daily use, the model needs to be updated and maintained constantly, which is time-consuming and laborious, reduces production efficiency, and has low accuracy. Therefore, there is still a lack of effective mixing uniformity decision tool for the mixing process of traditional Chinese medicine preparation. SUMMARY

[0004] Therefore, the present application provides a method for detecting the mixing uniformity of a mixture containing sodium sulfate or sodium sulfate extract, and the technical solution is as follows:

[0005] A method for detecting the mixing uniformity of a mixture containing sodium sulfate or sodium sulfate extract, comprising the following steps:

[0006] Sampling from the mixture containing sodium sulfate or sodium sulfate extract, and the sampling points are distributed at different positions of the mixture, and each sampling point corresponds to a sample N i ;

[0007] Respectively detecting the sample N i by ion chromatography, and determining the content of Na i in the sample N + ;

[0008] Calculating the relative standard deviation RSD of the content of Na i in each sample N + , and determining whether the mixture containing sodium sulfate or sodium sulfate extract is mixed uniformly according to the obtained relative standard deviation RSD.

[0009] In some embodiments, when the relative standard deviation RSD is less than or equal to 3%, it is determined that the mixture containing sodium sulfate or sodium sulfate extract is mixed uniformly.

[0010] In some embodiments, the sampling interval is 1m3 The mixed material corresponds to the distribution of at least three sampling points.

[0011] In some embodiments, the mixed material is an intermediate product for preparing a traditional Chinese medicine preparation, and the traditional Chinese medicine preparation is Da Chengqi Decoction, Tiaowei Chengqi Decoction, Daxianxian Decoction, Dahuang Mudan Decoction, Taohuachengqi Decoction, Jia Wei Tao Ren Chengqi Decoction, Shui Run Gao, Tongfu Runchang Decoction, Xinjia Huanglong Decoction, Dahuang Mudanpi Decoction, Xiesi Decoction, Fangfeng Tongsheng Powder, Quwei Chengqi Decoction, Jia Wei Xianglian Wan, Runchang Tongbian Decoction, Sanhuang Paishi Decoction, Paishi San, Xingshui Gao, Zengye Chengqi Decoction, Xiaotang San, Fuyang Jiming Decoction, Qingli Decoction, Qingmai Decoction, Mingmu Zhongtong Pill, Chaihu Jia Mangxie Decoction, Xianchuan Yulu Pill, Zaoshan Decoction, Shigao Yinzi, Bushen Xiaosh Decoction, San Yi Chengqi Decoction, or Shengma Gao.

[0012] In some embodiments, the sample N i is detected by ion chromatography to determine the content of Na i in the sample N + .

[0013] A sodium standard substance reference solution is prepared.

[0014] The sample N i is dissolved in a solvent to prepare a solution of the product to be tested sample N i .

[0015] The sodium standard substance reference solution and the solution of the sample N i to be tested are detected by ion chromatography, and the content of Na + is calculated according to the obtained chromatogram.

[0016] In some embodiments, the solvent is water.

[0017] In some embodiments, the detection condition of the ion chromatography detection includes that the eluent is a methanesulfonic acid aqueous solution.

[0018] In some embodiments, the concentration of methanesulfonic acid in the methanesulfonic acid aqueous solution is 20 mmol / L to 30 mmol / L.

[0019] In some embodiments, the flow rate of the methanesulfonic acid aqueous solution is 0.2 mL / min to 0.4 mL / min.

[0020] In some embodiments, the detection condition of the ion chromatography detection further includes that the guard column is Dionex IonPac CG12A.

[0021] In some embodiments, the detection condition of the ion chromatography detection further includes that the analysis column is Dionex IonPac CS12A.

[0022] In some embodiments, the detection conditions for the ion chromatography detection further include: the suppressor being a Dionex CSRS.

[0023] In some embodiments, the detection conditions for ion chromatography detection further include a column temperature of 25°C to 40°C.

[0024] In some embodiments, the detection conditions for ion chromatography detection further include: the detection cell temperature is 30°C to 40°C.

[0025] In some embodiments, the detection conditions for the ion chromatography detection further include: a suppressor current of 45mA to 49mA.

[0026] In some embodiments, the detection conditions for the ion chromatography detection further include a detector sensitivity of 4.5 μS to 5.5 μS.

[0027] In some embodiments, the detection conditions for the ion chromatography detection further include an injection volume of 5 μL to 20 μL.

[0028] Compared with traditional solutions, the present invention has the following advantages:

[0029] This invention innovatively proposes a method for detecting the mixing uniformity of mixtures containing Glauber's salt or Glauber's salt extract using ion chromatography. This method involves detecting the Nm of samples taken at different locations within the mixture. i ZhongNa + The content, based on Na + The relative standard deviation (RSD) of the content is used to determine whether the mixture containing Glauber's salt or its extract is uniformly mixed. Compared with traditional high-performance liquid chromatography (HPLC) and near-infrared spectroscopy, the detection method of this invention has higher accuracy, higher safety, and higher analytical efficiency. It can be applied to industrial production, thereby achieving rapid and accurate detection of the mixing uniformity in the mixing process of traditional Chinese medicine preparations and efficiently and conveniently monitoring the endpoint of mixing time. This provides a new strategy for quality control in the production process of traditional Chinese medicine preparations containing Glauber's salt. Attached Figure Description

[0030] To more clearly illustrate the technical solutions in the embodiments of this application and to more completely understand this application and its beneficial effects, the drawings used in the description of the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this application. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0031] Figure 1 This is the chromatogram for the specificity investigation of Example 1;

[0032] Figure 2Distribution of sampling points in the mixer (a is a front view, b is a top view, and c is a side view) for Example 2. DETAILED DESCRIPTION

[0033] The present application is further described in connection with the following specific examples. The present application can be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and fully convey the scope of the application to others skilled in the art.

[0034] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used in the description of the application herein is for describing particular embodiments only and is not intended to be limiting of the application.

[0035] In 1975, H. Small et al. proposed to use ion chromatography (IC) to determine trace amounts of anions and cations in the environment. Ion chromatography has been developed for more than forty years since then. Ion chromatography is mainly divided into three categories: ion exchange chromatography, ion pair chromatography, and ion exclusion chromatography. Among them, the separation method of ion exclusion chromatography is to use the spatial exclusion, Donnan exclusion, and adsorption between the stationary phase and the analyte. This separation method is suitable for the separation of organic acids or inorganic acids. The separation method of ion exchange chromatography is based on the exchange ion process between the mobile phase and the ion exchange group bonded on the substrate. It is suitable for the classification of organic anions and cations and inorganic anions and cations. The separation method of ion pair chromatography is based on the adsorption effect of the analyte on the separation column. The selectivity is focused on the composition and concentration of the mobile phase. In addition to adding organic modifiers, an appropriate amount of ion pair reagent can also be added. It is suitable for the separation of transition metal complexes and the separation of surface active anions and cations.

[0036] The present application innovatively proposes a method for detecting the mixing uniformity of a mixture containing mirabilite or mirabilite extract by ion chromatography. In one embodiment, the method for detecting the mixing uniformity of a mixture containing mirabilite or mirabilite extract comprises the following steps:

[0037] Sampling is taken from the mixture containing mirabilite or mirabilite extract. The sampling points are distributed at different positions of the mixture, and each sampling point corresponds to a sample N i ;

[0038] The samples N i are respectively detected by ion chromatography to determine the content of Na i in the samples N + .

[0039] The content of Na i in each sample N is calculated.+ the relative standard deviation RSD of the content of Na2SO3, according to the obtained relative standard deviation RSD, whether the mixture containing mirabilite or mirabilite extract is mixed uniformly is judged.

[0040] The mixing uniformity of the mixture containing mirabilite or mirabilite extract is detected by the above method, which can fully utilize the characteristics of ion chromatography, such as small sample injection volume, rapid analysis, high sensitivity, high selectivity, friendly experimental environment, small reagent pollution, and simple maintenance. Compared with traditional high performance liquid chromatography and near infrared spectroscopy, the detection method has higher accuracy, higher safety factor, and high analysis efficiency, and can be applied to industrial production, so that the mixing uniformity of the mixing process of the traditional Chinese medicine preparation containing mirabilite is quickly and accurately detected, and the end point of the mixing time is efficiently and conveniently monitored. A new strategy is provided for quality control of the production process of the traditional Chinese medicine preparation containing mirabilite.

[0041] Due to the influence of the quality fluctuation of the traditional Chinese medicine decoction pieces, after the traditional Chinese medicine decoction pieces are extracted, concentrated and dried into powder, there is a certain difference in the yield, and a proper amount of excipient needs to be added to adjust the total amount to ensure the consistency of the clinical application dose. The mixture in the embodiment can refer to the mixture of the traditional Chinese medicine extract and the excipient. In addition, if different traditional Chinese medicine ingredients are involved in the traditional Chinese medicine preparation, after different traditional Chinese medicine decoction pieces are extracted, concentrated and dried into powder, the mixture also needs to be fully mixed to ensure the consistency of the quality of the traditional Chinese medicine preparation. The mixture in the embodiment can also refer to the mixture between different traditional Chinese medicine extracts.

[0042] The mixture involved in the embodiment is an intermediate product for preparing a traditional Chinese medicine preparation, and the traditional Chinese medicine preparation is Da Chengqi Decoction, Tiaowei Chengqi Decoction, Daguanyan Decoction, Taohuochengqi Decoction, Jia Wei Tao Ren Chengqi Decoction, Shui Run Gao, Tong Fu Run Chang Decoction, Xin Jia Huang Long Decoction, Dahuang Mudan Decoction, Xiepi Decoction, Fangfeng Tongsheng Powder, Quai Chengqi Decoction, Jia Wei Xianglian Wan, Run Chang Tong Bian Decoction, Sanhuang Pai Shi Decoction, Pai Shi San, Xing Shui Gao, Zeng Ye Chengqi Decoction, Xiaotang San, Fuyang Jiming Decoction, Qingli Decoction, Qingmai Decoction, Mingmu Zhongtong Pill, Chaihu Jia Mangxiao Decoction, Xianchuan Yulu Pill, Zaoshan Decoction, Shigao Yinzi, Bushen Xiaoshi Decoction, San Yi Chengqi Decoction or Shengma Gao.

[0043] In the embodiment, according to the sample N i the relative standard deviation RSD of the content of Na + of Na2SO3, whether the mixture containing mirabilite or mirabilite extract is mixed uniformly is judged.

[0044] Optionally, when the relative standard deviation RSD is less than or equal to 3%, it is judged that the mixture containing mirabilite or mirabilite extract is mixed uniformly.

[0045] Optionally, 1 m 3The mixture is distributed with at least three sampling points. For example, there may be 3, 6, 9, 12, or 15 sampling points. Understandably, the sampling points in this embodiment can be evenly distributed at different locations in the mixture, depending on the actual situation.

[0046] In this embodiment, the mixing uniformity of the mixture containing sodium sulfate or sodium sulfate extract is tested. According to the inventors' research, Na... + The content of sodium sulfate and its extract was relatively high in samples containing sodium sulfate. Ion chromatography was used to detect N in samples from each sampling point. i Na in + The content of Na helps to make the test results more accurate. + The detection is not easily affected by other components in the mixture.

[0047] In this embodiment, an ion chromatography method for detecting Na can be constructed first. + The characteristic spectrum of the content, and then the N content of the test sample. i Na in + The content was tested.

[0048] Optionally, for the sample N i Ion chromatography was performed to determine the N content of the sample. i ZhongNa + The content includes the following steps:

[0049] Preparation of sodium standard reference solution;

[0050] Dissolve sample N in solvent i Product sample N to be tested i Solution;

[0051] The sodium standard reference solution and the sample N to be tested i The solution was subjected to ion chromatography detection, and the Na content was calculated based on the obtained chromatogram. + The content of.

[0052] Optionally, the method for preparing a sodium standard reference solution includes the following steps: adding water to a sodium composition analysis standard in water.

[0053] Optionally, the solvent is water, and the aqueous sample N is used. i .

[0054] Optionally, when sample N i When the sample is the Glauber's salt extract to be tested, N is calculated per 0.2g sample. i Add 10mL to 30mL of water accordingly; when sample N i When the sample is sodium sulfate, N is 0.2g per sample. i Add 10mL to 30mL of water accordingly.

[0055] Optionally, the detection condition of the ion chromatography detection comprises: the eluent is a methanesulfonic acid aqueous solution.

[0056] Optionally, the concentration of the methanesulfonic acid in the methanesulfonic acid aqueous solution is 20mmol / L-30mmol / L.

[0057] Optionally, the flow rate of the methanesulfonic acid aqueous solution is 0.2mL-0.4mL per minute.

[0058] Optionally, the detection condition of the ion chromatography detection further comprises: the guard column is Dionex IonPac CG12A. Further optionally, the specification is: inner diameter 3mm, column length 30mm, and packing particle size 5μm.

[0059] Optionally, the detection condition of the ion chromatography detection further comprises: the analytical column is Dionex IonPac CS12A. Further optionally, the specification is: inner diameter 3mm, column length 150mm, and packing particle size 5μm.

[0060] Optionally, the detection condition of the ion chromatography detection further comprises: the suppressor is Dionex CSRS. Further optionally, the specification is: CERS-2mm.

[0061] Optionally, the detection condition of the ion chromatography detection further comprises: the column temperature is 25℃-40℃.

[0062] Optionally, the detection condition of the ion chromatography detection further comprises: the detection cell temperature is 30℃-40℃.

[0063] Optionally, the detection condition of the ion chromatography detection further comprises: the suppressor current is 45mA-49mA.

[0064] Optionally, the detection condition of the ion chromatography detection further comprises: the detector sensitivity is 4.5μS-5.5μS.

[0065] Optionally, the detection condition of the ion chromatography detection further comprises: the injection volume is 5μL-20μL.

[0066] Example 1: Construction of characteristic pattern of ion chromatography detection of content of Na +

[0067] 1. Instruments and reagents

[0068] 1.1 Instruments

[0069] ​Ion chromatograph (ICS-6000, Thermo Fisher Scientific); electronic balance (ME204E / 02, METTLER TOLEDO); ultrapure water machine (Milli-Q Direct, Merck, Germany).

[0070] 1.2 Reagents

[0071] Sodium standard substance (sodium component analysis standard substance in water, batch number: 20200615, National Defense Science and Technology Industry Applied Chemistry First Grade Metrological Station)

[0072] Taohuochengqi decoction extract and dextrin

[0073] Mix 1 part by weight of the Taohuochengqi decoction extract and 1 part by weight of dextrin to obtain a mixture, which is an intermediate product for preparing Taohuochengqi decoction.

[0074] 2. Methods and results

[0075] 2.1 Chromatographic conditions

[0076] The guard column was Dionex IonPac CG12A (3mm*30mm, 5μm); 2) the analysis column was Dionex IonPac CS12A (3mm*150mm, 5μm); 3) the suppressor was Dionex CSRS2mm; 4) the column temperature was 30℃; 5) the detection cell temperature was 35℃; 6) the suppressor current was 47mA; 7) the detector sensitivity was 5μS; 8) the injection volume was 5μL.

[0077] 2.2 Preparation of sodium standard substance reference solution

[0078] Take an appropriate amount of sodium standard substance, accurately weigh, add water to contain Na + 1μg sodium standard substance reference solution per 1mL.

[0079] 2.3 Preparation of test solution

[0080] Take an appropriate amount of the mixture, finely grind, accurately weigh about 0.2g into a volumetric flask, accurately add 20mL of water, shake thoroughly to dissolve, shake evenly, filter, and take the filtrate to obtain the test solution.

[0081] 3 Methodology investigation

[0082] 3.1 Investigation of specificity

[0083] Accurately pipette the blank solvent (water), the sodium standard substance reference solution under item “2.2” and the test solution under item “2.3” respectively, inject into the ion chromatograph according to the chromatographic conditions under item “2.1”, and the results are shown in Table 1. Figure 1 ​

[0084] From Figure 1 It can be seen that the test solution chromatography has the same chromatographic peak at the retention time corresponding to the sodium standard substance reference solution chromatography, and the blank solvent has no interference, indicating that the method has good specificity.

[0085] 3.2 Linear relationship investigation

[0086] An appropriate amount of sodium standard substance was precisely weighed, water was added to prepare a control mother liquor with a mass concentration of 500 μg·mL -1 of sodium, and the mother liquor was diluted with water to prepare a series of sodium standard substance reference solutions with different concentrations. The sample was injected into the ion chromatograph under the chromatographic conditions in item 2.1, and the chromatogram was recorded. The mass concentration of the sodium standard substance reference solution (μg·mL -1 ) was taken as the abscissa (X), and the peak area was taken as the ordinate (Y) for linear regression. The standard curve was drawn, and the linear regression equation of Na + was Y=5.1286X+1.2278 (r=0.9995), indicating that the linear relationship of Na + was good in the range of 2-500 μg·mL -1 .

[0087] 3.3 Precision investigation

[0088] The sodium standard substance reference solution under item 2.2 was precisely taken, and the sample was continuously injected into the ion chromatograph under the chromatographic conditions in item 2.1 for 6 times. The chromatogram was recorded, and the RSD was calculated according to the peak area of Na + . The results showed that the RSD of the peak area of Na + was less than 3.0%, indicating that the method had good precision.

[0089] 3.4 Stability investigation

[0090] The test solution under item 2.3 was precisely taken, and the sample was injected into the ion chromatograph under the chromatographic conditions in item 2.1 at 0, 2, 4, 8, 12, and 24 h. The chromatogram was recorded, and the RSD was calculated according to the peak area of Na + . The results showed that the RSD of the peak area of Na + was less than 3.0%, indicating that the method had good stability within 24 h.

[0091] 3.5 Reproducibility investigation

[0092] Six portions of the test solution under item 2.3 were precisely taken, and the sample was injected into the ion chromatograph under the chromatographic conditions in item 2.1. The chromatogram was recorded, and the RSD was calculated according to the peak area of Na + . The results showed that the RSD of the peak area of Na + was less than 3.0%, indicating that the method had good reproducibility.

[0093] 3.6 Investigation of sample loading recovery rate

[0094] Take the mixture with known Glauber's salt extract content, precisely take 9 portions, each 0.1 g, place in a conical flask with a plug, divide into 3 groups, precisely add sodium standard substance reference solution of low, medium and high concentrations respectively, prepare the sample solution according to the method under "2.3", inject into the ion chromatograph according to the chromatographic conditions under "2.1", calculate the sample loading recovery rate and RSD, and the results are shown in Table 1.

[0095] Table 1

[0096]

[0097] From Table 1, the average sample loading recovery rate of Na + is 100.71%, and the RSD is 2.91%, indicating that the method has good accuracy.

[0098] Example 2 Sample N i of the sample points + Determination of the content of Na

[0099] Into a 3m 3 mixer, add 1 weight portion of Taohuojia decoction extract and 1 weight portion of dextrin respectively, set the mixer speed to 15 revolutions per minute, and when the mixer is running for 5 minutes, 10 minutes, 15 minutes, 20 minutes, 25 minutes and 30 minutes, use a sampler to take samples at the sampling points. The sampling method is as follows: insert the sampler from the top of the mixer, take samples at the specified sampling points, and save the sample numbers.

[0100] In this example, the distribution of the sampling points in the mixer is shown in Figure 2 , where a is the front view of the distribution of sampling points S1-S9 in the mixer, b is the top view of the distribution of sampling points S1-S9 in the mixer, and c is the side view of the distribution of sampling points S1-S9 in the mixer. As can be seen from Figure 2 , the most difficult mixing sampling point is S2, the line connecting S1, S4 and S7 is an equilateral triangle, the vertical downward from S1 to the contact conical surface is S3, the middle point between S1 and S3 is S2, similarly, there are sampling points S5 and S6 downward from S4, and sampling points S8 and S9 downward from S7.

[0101] In this example, after sampling at sampling points S1-S9, take an appropriate amount of sample, grind finely, take about 0.2 g, precisely weigh, into a volumetric flask, precisely add 20 mL of water, shake thoroughly to dissolve, shake uniformly, filter, and take the filtrate, to obtain sample solutions N1-N9 to be tested.

[0102] Take the reference solution and the test sample solutions N1 to N9, and inject them into the ion chromatogram under the chromatographic conditions described in section "2.1" of Example 1. Record the chromatograms. Calculate the Na content of N1 to N9 using the external standard method. + The content is summarized in Table 2.

[0103] Table 2

[0104]

[0105] As shown in Table 2, with the extension of the mixing time of the mixer, the Na content in the samples at sampling points S1-S9 increases. + The RSD of the content gradually decreased, indicating that the above method can provide a feasible and accurate data basis for the mixing uniformity of the mixture, and can provide a basis and guidance for the detection of the mixing uniformity of mixtures containing Glauber's salt or Glauber's salt extract, thereby improving the level of product quality control.

[0106] In summary, the criterion for judging the mixing uniformity of mixtures containing Glauber's salt or Glauber's salt extract is: when sample N i ZhongNa + When the relative standard deviation (RSD) of the content is ≤3%, the mixture containing Glauber's salt or Glauber's salt extract is considered to be uniformly mixed. Among them, sample N... i The sampling points meet the following conditions: every 1m 3 The mixture has at least three sampling points distributed accordingly.

[0107] The above method is used to detect the mixing uniformity of mixtures containing Glauber's salt or Glauber's salt extract, and has the following advantages:

[0108] 1) The test method has a short cycle and high detection efficiency, and can quickly determine whether the mixture containing Glauber's salt or Glauber's salt extract is uniformly mixed, which meets the needs of modern enterprises for rapid and large-scale production.

[0109] 2) The sample preparation process is simple, does not involve organic or toxic reagents, and is green, environmentally friendly and pollution-free.

[0110] 3) Sodium standard substances are inexpensive and readily available, and the detection method has a low cost.

[0111] The technical features of the above embodiments can be combined in any way. For the sake of brevity, not all possible combinations of the technical features in the above embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0112] The above embodiments only express several implementation manners of the present application, and the description is more specific and detailed, but it should not be understood as a limitation on the scope of the patent. It should be noted that for ordinary skilled persons in the art, without departing from the concept of the present application, several modifications and improvements can be made, which are within the scope of protection of the present application. Therefore, the protection scope of the patent of the present application should be subject to the appended claims.

Claims

1. A method for detecting the mixing uniformity of a mixture containing Glauber's salt or a Glauber's salt extract, characterized by, The method comprises the following steps: A sodium standard substance reference solution is prepared; Sampling in the mixture containing mirabilite or mirabilite extract, the sampling points are distributed in different positions of the mixture, and each sampling point corresponds to a sample N i ; Dissolve sample N in solvent i , product under test sample N i solution; The sodium standard substance reference solution and the sample N to be measured are prepared according to the following steps. i The solution is detected by ion chromatography, and the content of Na is calculated according to the obtained chromatogram. + The sodium standard substance reference solution and the sample N to be measured are prepared according to the following steps. The N of each sample was calculated i The relative standard deviation RSD of the content of Na + According to the obtained relative standard deviation RSD, it is judged whether the mixture containing mirabilite or mirabilite extract is uniformly mixed. The detection conditions of the ion chromatography detection include: 1) the guard column is Dionex IonPac CG12A; 2) the analysis column is Dionex IonPac CS12A; 3) the suppressor is Dionex CSRS; 4) the column temperature is 25-40 DEG C; 5) the detection cell temperature is 30-40 DEG C; 6) the suppressor current is 45-49 mA; 7) the detector sensitivity is 4.5-5.5 muS; 8) the injection volume is 5-20 muL; and 9) the eluent is a methanesulfonic acid aqueous solution, wherein the concentration of methanesulfonic acid in the methanesulfonic acid aqueous solution is 20-30 mmol / L.

2. The detection method according to claim 1, characterized in that, When the relative standard deviation RSD is less than or equal to 3%, it is determined that the mixture containing mirabilite or mirabilite extract is uniformly mixed.

3. The detection method according to claim 2, characterized in that, Every 1 m 3 The mixture corresponds to a distribution of at least 3 sampling points.

4. The method of claim 1, wherein The mixture is an intermediate product for preparing a traditional Chinese medicine preparation, and the traditional Chinese medicine preparation is Da Chengqi Decoction, Tiaowei Chengqi Decoction, Da Xianxiong Decoction, Taohuochengqi Decoction, Jia Wei Tao Renchengqi Decoction, Shui Run Gao, Tong Fu Run Chang Decoction, Xin Jia Huang Long Decoction, Da Huang Mudan Decoction, Xieli Decoction, Fangfeng Tongsheng Powder, Quwei Chengqi Decoction, Jia Wei Xianglian Pill, Run Chang Tong Bian Decoction, Sanhuang Pai Shi Decoction, Pai Shi San, Xing Shui Gao, Zengye Chengqi Decoction, Xiaotang San, Fuyang Jiming Decoction, Qingli Decoction, Qingmai Decoction, Mingmu Zhiti Pill, Chaihu Jia Mangxie Decoction, Xianchuan Yulu Pill, Zaoshan Decoction, Shigao Yinzi, Bushen Xiaoshi Decoction, San Yi Chengqi Decoction or Shengma Gao.

5. The method of claim 1, wherein The solvent is water.

6. The method of claim 1, wherein The flow rate of the methanesulfonic acid aqueous solution is 0.2-0.4 mL / min.

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