Detecting method of content of vitamin K<2>(MK-7)

A detection method, vitamin technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of difficult operation, low extraction rate of active ingredients, long processing time, etc., to improve accuracy and reliability, and accurate and reliable detection results , The effect of simple detection method

Inactive Publication Date: 2019-04-23
CHENGUANG BIOTECH GRP HANDAN CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Determination of Vitamin K in Natto Extract by Reversed-Phase High Performance Liquid Chromatography 2 (35) Content" ("China Drug Standards" 2010 Volume 11 No. 4 Issue 287) The sample treatment method and chromatographic conditions reported in the literature can not effectively extract the trace amount of menadione (MK-7 ), and can not effectively separate the purpose peak from the impurity peak; the inventor of the present invention utilizes the method in the above-mentioned literature to carry out vitamin K soft capsule, calcium vitamin D vitamin K soft capsule and calcium vitamin D vitamin K chewable tablet etc. 2 Determination of (MK-7) content, the measurement results show that vitamin K 2 (MK-7) The resolution of the main peak is less than 1.5, which cannot effectively separate the target peak from the impurity peak
"A Vitamin K 2 (MK-7) Assay method for content of vitamin K disclosed in "(CN104458990) 2 (MK-7) content detection method extracts the content of active ingredients from different calcium preparations on the low side, and the amount of sample weighing has a certain influence on the constant volume, which is difficult to operate and takes a long time to process; the inventor of the present invention adopts the above-mentioned Methods: Calcium, vitamin D, vitamin K softgels and calcium, vitamin D, vitamin K chewable tablets, etc. 2 Determination of (MK-7) content, the measurement results show that the extraction rate of active ingredients is extremely low, which in turn leads to the determination of vitamin K 2 The content of (MK-7) is 50% or even more lower than the actual content; in addition, the active ingredient in the sample to be tested prepared by this method is low, for the composite preparation containing more auxiliary materials such as using soybean oil, corn Oil or other vegetable oils cannot effectively separate the impurity peaks in the excipients from the target peaks

Method used

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  • Detecting method of content of vitamin K&lt;2&gt;(MK-7)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] 1. Sample to be tested

[0050] 1.1 Vitamin K soft capsule: batch number: VK180001, production unit: Chenguang Biotechnology Group Handan Co., Ltd.

[0051] 2. Reagents and Materials

[0052] 2.1 Isopropanol (analytical pure)

[0053] 2.2 Petroleum ether (analytical pure)

[0054] 2.3 Methanol (analytical pure)

[0055] 2.3 Acetonitrile (chromatographically pure)

[0056] 2.4 Methanol (chromatographically pure)

[0057] 3. Chromatographic conditions

[0058] 3.1 Chromatographic column: Amethyst C18-H (4.6×150mm, 5μm);

[0059] 3.2 Mobile phase: use acetonitrile as mobile phase A, methanol as mobile phase B, and carry out gradient elution according to the regulations in the table below;

[0060]

[0061] 3.3 Mobile phase flow rate: 0.8mL / min;

[0062] 3.4 Column temperature: 40°C;

[0063] 3.5 Injection volume: 10μL;

[0064] 3.6 Detection wavelength: UV visible 254nm;

[0065] 4. Analysis steps

[0066] 4.1 Preparation of reference substance solution: Acc...

Embodiment 2

[0080] 1. Sample to be tested

[0081] 1.1 calcium vitamin D vitamin K soft capsule, batch number: KGR180001, production unit: Chenguang Biotechnology Group Handan Co., Ltd.

[0082] 2. Reagents and Materials

[0083] 2.1 n-Hexane (analytical pure)

[0084] 2.2 Isopropanol (analytical pure)

[0085] 2.3 Petroleum ether (analytical pure)

[0086] 2.4 Acetonitrile (chromatographically pure)

[0087] 2.5 methanol (chromatographically pure)

[0088] 3. Chromatographic conditions

[0089] 3.1 Chromatographic column: SPOLAR C18 (4.6×250mm, 5μm);

[0090] 3.2 Mobile phase: use acetonitrile as mobile phase A, methanol as mobile phase B, and carry out gradient elution according to the regulations in the table below;

[0091]

[0092] 3.3 Mobile phase flow rate: 1.0mL / min;

[0093] 3.4 Column temperature: 30°C;

[0094] 3.5 Injection volume: inject 10 μL of the reference substance solution, inject 20 μL of the sample to be tested;

[0095] 3.6 Detection wavelength: UV visib...

Embodiment 3

[0111] 1. Sample to be tested

[0112] 1.1 Calcium Vitamin D and Vitamin K Chewable Tablets, batch number: KGJ180002, production unit: Chenguang Biotechnology Group Handan Co., Ltd.

[0113] 2. Reagents and Materials

[0114] 2.1 Isopropanol (analytical pure)

[0115] 2.2 Cyclohexane (analytical pure)

[0116] 2.3 Acetonitrile (analytical pure)

[0117] 2.4 Acetonitrile (chromatographically pure)

[0118] 2.5 absolute ethanol (chromatographically pure)

[0119] 3. Chromatographic conditions

[0120] 3.1 Chromatographic column: Shim-pack GIST C18 (4.6×250mm, 5μm);

[0121] 3.2 Mobile phase: use acetonitrile as mobile phase A, methanol as mobile phase B, and carry out gradient elution according to the regulations in the table below;

[0122]

[0123] 3.3 Mobile phase flow rate: 1.5mL / min;

[0124] 3.4 Column temperature: 25°C;

[0125] 3.5 Injection volume: inject 10 μL of the reference substance solution, inject 20 μL of the sample to be tested;

[0126] 3.6 Detect...

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Abstract

The invention discloses a detecting method of the content of vitamin K<2>(MK-7), and belongs to the technical field of compound content detecting. The detecting method comprises the following processes of A, pretreatment of a sample, B, preparation of a reference substance solution, C, preparation of a to-be-detected solution, D, detection of the standard reference substance solution by using a high performance liquid chromatography technology and E, calculation of the content C of the vitamin K<2>(MK-7) in the to-be-detected sample according to an external standard method. According to the detecting method of the content of the vitamin K<2>(MK-7), the extraction rate of efficacy components is improved, the detecting result is precise and reliable, and the detecting method is convenient and efficient; the detecting method of the content of the vitamin K<2>(MK-7) has wide application range, and can be used for rapid detecting of the content of health food, medicine, plain food or premixproducts and the like containing menaquinone-7 (MK-7).

Description

technical field [0001] The invention relates to the field of health food or medicine detection, in particular to a product containing vitamin K 2 (MK-7) Determination method for the content of menadione active ingredients in compound preparations such as soft capsules, tablets, and granules. Background technique [0002] Vitamin K 2 , also known as menadione, is a light yellow crystal, mainly synthesized by intestinal bacteria; it is a class composed of a menaquinone mother ring and an isoprene side chain at the C-3 position of the mother ring Fat-soluble compound with quinone structure. According to the number of isoprene units on the side chain, menadione is divided into 14 types, represented by MK-n, all of which are heat-resistant, but sensitive to light and alkali. Menaquinone (MK-7) is a member of MK-n, and its side chain contains 7 isoprene units. [0003] Menadione (MK-7) has a long half-life and is stable in blood, so it is a very important cofactor for mammals ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/14
CPCG01N30/02G01N30/06G01N30/14G01N2030/047
Inventor 王新艳史晓彤程永科薛强
Owner CHENGUANG BIOTECH GRP HANDAN CO LTD
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