阅读说明：本技术 一种通窍鼻炎颗粒溶出度测定法 (Method for determining dissolution rate of orifice-opening rhinitis particles ) 是由 李珺 张律 汤海 詹祥静 黄岂庸 毛洁 张平 杜江 文佳燕 于 2019-01-31 设计创作，主要内容包括：本发明提供了一种通窍鼻炎颗粒溶出度测定法。本发明的通窍鼻炎颗粒溶出度测定法,构建了溶出度测定的条件,确定了溶出介质、搅拌桨转速、取样时间。相较于《中国药典》2015年版一部项下通窍鼻炎片质量测定方法,本发明完善了通窍鼻炎制剂的检测项目,为通窍鼻炎颗粒的质量判定提供了新方法。(The invention provides a dissolution testing method of orifice-opening rhinitis particles. The method for measuring the dissolution rate of the orifice-opening rhinitis particles constructs the condition for measuring the dissolution rate and determines the dissolution medium, the rotating speed of the stirring paddle and the sampling time. Compared with the method for measuring the quality of the orifice-opening rhinitis tablets under the item of the first edition of Chinese pharmacopoeia 2015, the method improves the detection items of the orifice-opening rhinitis preparation and provides a new method for judging the quality of the orifice-opening rhinitis particles.)

1. A method for measuring the dissolution rate of orifice-opening rhinitis particles is characterized in that: the method comprises the following operation steps:

1) preparation of control solutions: dissolving imperatorin in methanol to obtain reference substance;

2) preparation of a test solution: taking orifice-opening rhinitis granules, taking a sodium dodecyl sulfate solution as a dissolution medium, performing constant temperature, uniform speed and timed dissolution, taking a dissolution liquid, centrifuging, and taking the supernatant as a test solution;

3) and (3) measuring the dissolution amount: respectively sucking the reference solution and the test solution, injecting into a liquid chromatograph, and calculating the dissolution amount of imperatorin in the resuscitation and rhinitis granules; the chromatographic conditions are as follows: a chromatographic column: c18 column, mobile phase: methanol is used as a mobile phase A phase, water is used as a mobile phase B phase, and isocratic elution is carried out: phase A: phase B54: 46.

2. the assay according to claim 1, characterized in that: the solution concentration of the imperatorin reference substance in the step 1) is 1.5 mug/ml.

3. The assay according to claim 1, characterized in that: the mass-to-volume ratio of the orifice-opening rhinitis particles to the sodium dodecyl sulfate solution in the step 2) is 2:500 g/ml; the concentration of the sodium dodecyl sulfate solution is 0.1%.

4. The assay according to claim 1, characterized in that: the constant temperature in the step 2) is that the temperature of the dissolution medium is constant at 37 +/-0.5 ℃; the uniform speed is that the rotating speed of the stirring paddle is set to be 50 r/min; the timing is that the dissolution time is 45 min; the dosage of the dissolution liquid is 20 ml; the speed of centrifugation is 12000r/min, and the time is 10 min.

5. The assay according to claim 1, characterized in that: and 3) respectively sucking the reference solution and the test solution into 20 mul.

6. The assay according to claim 1, wherein the C18 column of step 3) is Inertsil ODS-2, 4.6 × 150mm 5um or Shim-pack VP-ODS, 4.6 × 150mm 5 um.

7. The assay according to claim 1, characterized in that: the detection wavelength of the chromatographic conditions in the step 3) is 248nm, the column temperature is 35 ℃, the flow rate is 1ml/min, and the number of theoretical plates is not less than 3000 calculated according to the imperatorin peak.

8. The assay according to claim 1, characterized in that: and 3) the limit of the dissolution amount of the imperatorin in the granules for relieving stuffiness and rhinitis is 70%.

Technical Field

The invention relates to a method for measuring the dissolution rate of orifice-opening rhinitis particles.

Background

The rhinitis-treating granule is prepared with 6 kinds of Chinese medicinal materials including astragalus root, ledebouriella root, cocklebur fruit, magnolia flower, white atractylodes rhizome, etc. and through decoction, filtering, decompression concentration to obtain clear paste, mixing with crushed white atractylodes rhizome and crushed dahurian angelica root, drying and crushing.

In 2015, the dissolution rate of the suspension particles should be checked according to the general rule '0104 granules' in the fourth part of the Chinese pharmacopoeia. However, no method for checking the dissolution rate of orifice-opening rhinitis particles is reported at present, and no dissolution rate checking method is listed in the method for measuring the quality of orifice-opening rhinitis tablets under the item of the first part of the 2015 in the Chinese pharmacopoeia.

Disclosure of Invention

In order to solve the problems, the invention provides a method for measuring the dissolution rate of orifice-opening rhinitis particles, which is characterized by comprising the following steps: the method comprises the following operation steps:

1) preparation of control solutions: dissolving imperatorin in methanol to obtain reference substance;

2) preparation of a test solution: taking orifice-opening rhinitis granules, taking a sodium dodecyl sulfate solution as a dissolution medium, performing constant temperature, uniform speed and timed dissolution, taking a dissolution liquid, centrifuging, and taking the supernatant as a test solution;

3) and (3) measuring the dissolution amount: respectively sucking the reference solution and the test solution, injecting into a liquid chromatograph, and calculating the dissolution amount of imperatorin in the resuscitation and rhinitis granules; the chromatographic conditions are as follows: a chromatographic column: c18 chromatographic column, mobile phase methanol-water (54: 46).

Further, the concentration of the imperatorin reference solution in the step 1) is 1.5 mu g/ml.

Further, the mass-volume ratio of the resuscitation inducing rhinitis particles in the step 2) to the sodium dodecyl sulfate solution is 2:500 g/ml.

Further, the sodium lauryl sulfate solution has a concentration of 0.1%.

Further, the constant temperature in the step 2) is that the temperature of the dissolution medium is constant at 37 ℃ +/-0.5 ℃; the uniform speed is that the rotating speed of the stirring paddle is set to be 50 r/min; the timing is that the dissolution time is 45 min; the dosage of the dissolution liquid is 20 ml; the speed of centrifugation is 12000r/min, and the time is 10 min.

Further, the volumes of the reference solution and the test solution in step 3) are respectively sucked to be 20 μ l.

Further, the C18 chromatographic column in the step 3) is Inertsil ODS-2, 4.6 × 150mm 5um or Shim-pack VP-ODS, 4.6 × 150mm 5 um.

Further, the detection wavelength of the chromatographic conditions in the step 3) is 248nm, the column temperature is 35 ℃, the flow rate is 1ml/min, and the number of theoretical plates is not less than 3000 according to the calculation of imperatorin peak.

Further, the limit of the dissolution amount of the imperatorin in the particles for relieving stuffy nose and rhinitis in the step 3) is 70%.

The invention relates to a dissolution testing method of orifice-opening rhinitis particles, which constructs the conditions of dissolution testing and determines dissolution media, the rotating speed of a stirring paddle and sampling time. Improves the detection items of the orifice-opening rhinitis preparation and provides a new method for judging the quality of the orifice-opening rhinitis granules.

Obviously, many modifications, substitutions, and variations are possible in light of the above teachings of the invention, without departing from the basic technical spirit of the invention, as defined by the following claims.

The present invention will be described in further detail with reference to the following examples. This should not be understood as limiting the scope of the above-described subject matter of the present invention to the following examples. All the technologies realized based on the above contents of the present invention belong to the scope of the present invention.

Drawings

FIG. 1 high performance liquid chromatogram of blank solution

FIG. 2 high performance liquid chromatogram of negative control solution

FIG. 3 high performance liquid chromatogram of control solution

FIG. 4 high performance liquid chromatogram of test solution

Detailed Description

Instrument and reagent

The instrument comprises the following steps: high performance liquid chromatograph, ultrasonic cleaner, high speed centrifuge, dissolution tester and electronic balance.

Reagent: methanol (chromatographically pure), sodium dodecyl sulfate (analytically pure), ultrapure water.

Comparison products: imperatorin.

Sample preparation: tongqiao Biyan Keli (rhinitis treating granule).

The reagents, devices and samples used in the embodiments of the present invention are all known products, and are obtained by purchasing commercially available products