阅读说明：本技术 一种九制黄精的质量检测方法 (Quality detection method of nine-process sealwort ) 是由 胡昌江 陈志敏 胡麟 于 2018-06-28 设计创作，主要内容包括：本发明提供了九制黄精的单糖检测方法,它包括如下操作步骤：1)对照品溶液制备；2)供试品溶液制备；3)分别吸取对照品溶液和供试品溶液注入高效液相色谱仪,检测。本发明还提供了九制黄精的质量检测方法。本发明九制黄精的单糖检测方法可以准确检测其单糖含量,在九制黄精质量检测方法增加单糖检测使得质量检测体系更加完善,应用前景良好。(The invention provides a monosaccharide detection method of nine-process sealwort, which comprises the following operation steps: 1) preparing a reference substance solution; 2) preparing a test solution; 3) respectively sucking the reference solution and the sample solution, injecting into a high performance liquid chromatograph, and detecting. The invention also provides a quality detection method of the nine-process sealwort. The monosaccharide detection method for the Jiuzhi sealwort can accurately detect the monosaccharide content of the Jiuzhi sealwort, and the monosaccharide detection is added in the quality detection method for the Jiuzhi sealwort, so that the quality detection system is more perfect, and the application prospect is good.)

1. A monosaccharide detection method of nine-process sealwort is characterized by comprising the following steps: the method comprises the following operation steps:

1) preparation of a reference solution: dissolving D-glucose as reference substance, and derivatizing with 1-phenyl-3-methyl-5-pyrazolone to obtain reference substance solution;

2) preparing a test solution: taking a nine-process polygonatum medicinal material to be detected, extracting, and deriving by adopting 1-phenyl-3-methyl-5-pyrazolone to obtain a test solution;

3) respectively sucking the reference solution and the test solution, injecting into a high performance liquid chromatograph, and detecting under the following chromatographic conditions:

a chromatographic column: octadecylsilane chemically bonded silica is used as a filling agent; detection wavelength: 250 nm; mobile phase: 0.02 mol. L^-1A mixed solution of ammonium acetate solution and acetonitrile.

2. The detection method according to claim 1, characterized in that: the dissolving in the step 1) is adding water for dissolving.

3. The detection method according to claim 1, characterized in that: the steps of 1-phenyl-3-methyl-5-pyrazolone derivation in the step 1) and the step 2) are as follows:

taking a solution to be derived, adding a sodium hydroxide solution, adding a methanol solution of 1-phenyl-3-methyl-5-pyrazolone, uniformly mixing, reacting in a dark place, adding a hydrochloric acid solution for neutralization, adding trichloromethane, uniformly mixing, centrifuging, and removing a trichloromethane layer to obtain a water layer.

4. The detection method according to claim 2, characterized in that: adding 100 mu L of sodium hydroxide solution, 100 mu L of 1-phenyl-3-methyl-5-pyrazolone methanol solution, 100 mu L of hydrochloric acid solution and 1mL of chloroform into every 100 mu L of solution to be derived; the concentration of the sodium hydroxide solution is 0.6 mol.L^-1The concentration of the methanol solution of the 1-phenyl-3-methyl-5-pyrazolone is 0.5 mol.L^-1The concentration of the hydrochloric acid solution is 0.3 mol.L^-1。

5. The detection method according to claim 1, characterized in that: the extraction method in the step 2) comprises the following steps: extracting rhizoma Polygonati with water.

6. The detection method according to claim 5, characterized in that: adding water 50w/v (g/ml) times of the processed rhizoma Polygonati into the processed rhizoma Polygonati, ultrasonic extracting, cooling, adding water to supplement the lost mass, filtering, and collecting the filtrate.

7. The detection method according to claim 1, characterized in that: in step 3), the chromatographic column used is Welch

8. The detection method according to claim 1, characterized in that: in the step 3), the column temperature is 30 ℃; and/or a flow rate of 1 mL/min^-1。

9. A quality detection method of nine-process sealwort is characterized in that: it includes:

(1) measuring the extract;

(2) measuring the content of polysaccharide;

(3) measuring moisture;

(4) measuring total ash content;

(5) monosaccharide assay according to any one of claims 1 to 8.

10. A preparation method of nine-process sealwort is characterized by comprising the following steps: the method comprises the following steps: collecting cut rhizoma Polygonati decoction pieces, adding black bean juice, moistening for 3 hr, steaming at 105 deg.C for 1 hr, drying at 70 deg.C for 5 hr, and repeating for 9 times.

Technical Field

The invention particularly relates to a quality detection method of nine-process sealwort.

Background

Polygonatum sibiricum is a plant belonging to the genus Polygonatum of the family Liliaceae, and is obtained from dried rhizome of Polygonatum kingianum Coll et Hemsl, Polygonatum sibiricum Red or Polygonatum cyrtonema Hua, recorded in Ming Yi Bie Lu. Most of the herbs are called "rheum officinale essence", "polygonatum odoratum" and "polygonatum zingiberense" according to their shapes. Sweet in nature and taste and mild in nature. It enters spleen, lung and kidney meridians. Has effects in invigorating qi, nourishing yin, invigorating spleen, moistening lung, and invigorating kidney. Can be used for treating deficiency of spleen-stomach qi, asthenia, stomach yin deficiency, xerostomia, cough with little appetite, lung deficiency, cough with excessive consumption, hemoptysis, essence and blood deficiency, soreness of waist and knees, premature gray hair, and internal heat diabetes, and is a commonly used Chinese medicinal tonic. Researches find that the sealwort has the functions of reducing blood pressure, blood sugar, blood fat and tumor. Tang dynasty poetry Dufu describes that rhizoma polygonati, namely rhizoma polygonati for removing white hair and removing snow and ice for other people, fully shows that rhizoma polygonati can make human skin smooth, skin color ruddy and hair black and bright, and has the effects of prolonging life, preserving essence and beautifying after eating rhizoma polygonati. In the early stage, the nine-process sealwort is optimized and applied for patent protection.

However, the quality standard research of the nine-process sealwort is still incomplete, the quality of the nine-process sealwort cannot be comprehensively controlled, and further improvement is needed.

Disclosure of Invention

The invention combines the component change characteristics in the nine-process sealwort steaming process, newly adds monosaccharide as one of the quality control standards, and establishes a quality standard system which better accords with the nine-process sealwort.

Firstly, the invention provides a monosaccharide detection method for nine-process sealwort, which comprises the following operation steps:

1) preparation of a reference solution: dissolving D-glucose as reference substance, and derivatizing with 1-phenyl-3-methyl-5-pyrazolone to obtain reference substance solution;

2) preparing a test solution: taking a nine-process polygonatum medicinal material to be detected, extracting, and deriving by adopting 1-phenyl-3-methyl-5-pyrazolone to obtain a test solution;

3) respectively sucking the reference solution and the test solution, injecting into a high performance liquid chromatograph, and detecting under the following chromatographic conditions:

a chromatographic column: octadecylsilane chemically bonded silica is used as a filling agent; detection wavelength: 250 nm; mobile phase: 0.02 mol. L^-1A mixed solution of ammonium acetate solution and acetonitrile.

The dissolving in the step 1) is adding water for dissolving.

The steps of 1-phenyl-3-methyl-5-pyrazolone derivation in the step 1) and the step 2) are as follows:

taking a solution to be derived, adding a sodium hydroxide solution, adding a methanol solution of 1-phenyl-3-methyl-5-pyrazolone, uniformly mixing, reacting in a dark place, adding a hydrochloric acid solution for neutralization, adding trichloromethane, uniformly mixing, centrifuging, and removing a trichloromethane layer to obtain a water layer.

Preferably, every 100 mu L of the solution to be derived is added with 100 mu L of sodium hydroxide solution, 100 mu L of 1-phenyl-3-methyl-5-pyrazolone methanol solution, 100 mu L of hydrochloric acid solution and 1mL of trichloromethane; the concentration of the sodium hydroxide solution is 0.6 mol.L^-1The concentration of the methanol solution of the 1-phenyl-3-methyl-5-pyrazolone is 0.5 mol.L^-1The concentration of the hydrochloric acid solution is 0.3 mol.L^-1。

The extraction method in the step 2) comprises the following steps: extracting rhizoma Polygonati with water. Preferably, the nine-process rhizoma polygonati medicinal material is taken, water 50w/v (g/ml) times of the medicinal material is added, ultrasonic extraction is carried out, cooling is carried out, water is used for complementing lost mass, filtration is carried out, and subsequent filtrate is taken.

In step 3), the chromatographic column used is Welch

XB。

In the step 3), the column temperature is 30 ℃; and/or a flow rate of 1 mL/min^-1。

The invention also provides a quality detection method of the nine-process sealwort, which comprises the following steps:

(1) measuring the extract;

(2) measuring the content of polysaccharide;

(3) measuring moisture;

(4) measuring total ash content;

(5) monosaccharide determinations were performed as described previously.

The invention also provides a preparation method of the nine-process sealwort, which comprises the following steps: collecting cut rhizoma Polygonati decoction pieces, adding black bean juice, moistening for 3 hr, steaming at 105 deg.C for 1 hr, drying at 70 deg.C for 5 hr, and repeating for 9 times.

The invention provides a detection method of Jiuzhi sealwort monosaccharide by combining the component change characteristics in the Jiuzhi sealwort steaming process, establishes a quality standard system which is more in line with the Jiuzhi sealwort by taking the monosaccharide as one of the quality control standards of the Jiuzhi sealwort, and provides a novel preparation method of the Jiuzhi sealwort.

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 is a graph of the results of a system suitability test.

Fig. 2 different mobile phase investigation, above: acetonitrile-water; the following: acetonitrile-ammonium acetate.

Detailed Description