CN105467035A - Method for detecting macromolecular substances in Shenxiong glucose injection - Google Patents
Method for detecting macromolecular substances in Shenxiong glucose injection Download PDFInfo
- Publication number
- CN105467035A CN105467035A CN201510973210.3A CN201510973210A CN105467035A CN 105467035 A CN105467035 A CN 105467035A CN 201510973210 A CN201510973210 A CN 201510973210A CN 105467035 A CN105467035 A CN 105467035A
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- Prior art keywords
- glucose injection
- dextran
- reference substance
- need testing
- macromolecular substances
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
Abstract
The invention discloses a method for detecting macromolecular substances in a Shenxiong glucose injection, comprising the following steps: (1) establishing the following chromatographic conditions; (2) preparing a standard substance solution; (3) preparing a test article solution; (4) measuring: respectively taking 5 mu. L of the standard substance solution prepared in step (2) and 5 mu. L of the test article solution prepared in step (3), and performing HPLC-ELSD detection; if appearance time in a test article color spectrum is greater than the impurity peak of a dextran D4 reference substance, determining that macromolecules exist, and calculating the ratio of a peak area greater than the impurity peak of the dextran D4 reference substance according to peak area percentage. The ratio of the macromolecular substances in the Shenxiong glucose injection is measured by adopting an efficient liquid chromatography, the content of the macromolecules in the Shenxiong glucose injection can be effectively detected, the sample repeatability is good, the accuracy degree is high, and the accuracy and the effectiveness of a detection result can be ensured. The quality standard of the Shenxiong glucose injection is improved, and safety detection and measurement on the Shenxiong glucose injection are strengthened.
Description
Technical field:
The present invention relates to the detection technique field of ginseng rhizome of chuanxiong glucose injection, in particular to macromolecular substances detection method in ginseng rhizome of chuanxiong glucose injection, do not relate in method primary standard of the present invention, belong to newly-increased detection method, it detects sample favorable reproducibility, and accuracy is high.
Background technology:
Macromolecular substances is the material that molecular weight is larger.Explain there is different materials from biological and chemical two aspects.Biological aspect mainly contains polysaccharide, protein, nucleic acid etc.The chemistry aspect mainly macromolecular compound such as superpolymer.Do not mention in large molecule primary standard in current ginseng rhizome of chuanxiong glucose injection and how to detect.
Summary of the invention:
Technical matters solved by the invention provides a kind of for the leak existing for ginseng rhizome of chuanxiong glucose injection test item and detects accurately simultaneously in guarantee, what facilitate again inspection work carries out macromolecular substances detection method in ginseng rhizome of chuanxiong glucose injection, the method increase the quality standard of ginseng rhizome of chuanxiong glucose injection, strengthen ginseng rhizome of chuanxiong glucose injection agent security detection management.
Technical matters pin solved by the invention can be achieved through the following technical solutions:
Macromolecular substances detection method in ginseng rhizome of chuanxiong glucose injection, is characterized in that, be made up of following steps:
(1) following chromatographic condition is set up:
Chromatographic condition: gel chromatographic columns, column temperature 25 ~ 50 DEG C, mobile phase: 1 ~ 7mmol/L ammonium acetate, flow velocity is 0.5 ~ 1.5mL/min, the drift tube temperature 40 ~ 60 DEG C of setting evaporative light dispersion dispersion, dry gas flow velocity 0.2 ~ 1.2L/min, sample size: 5 μ L;
(2) preparation of standard solution:
Precision takes the dextran D4 reference substance 20mg being dried to constant weight at 80 DEG C, accurately weighed, puts in 5ml measuring bottle, adds water and make dissolving in right amount and be diluted to scale, shake up, and obtains every 1mL containing dextran D4 reference substance 4mg;
(3) preparation of need testing solution:
Get the ginseng rhizome of chuanxiong glucose injection of different lot number respectively, cross 0.45 μm of miillpore filter, obtain need testing solution;
(4) measure:
Get standard solution prepared by step (2) and each 5 μ L of need testing solution prepared by step (3) respectively, detect through HPLC-ELSD; In test sample chromatogram, appearance time is greater than dextran D4 reference substance impurity peaks is large molecule, amasss percentage calculation be greater than dextran D4 reference substance impurity peaks sharp side and amass accounting by sharp side.
The present invention adopts high effective liquid chromatography for measuring to join the accounting of macromolecular substances in rhizome of chuanxiong glucose injection, effectively can detect macromolecular content in ginseng rhizome of chuanxiong glucose injection, and sample repeatability is good, accuracy is high, and more can ensure accuracy, the validity of testing result.Invention increases the quality standard of ginseng rhizome of chuanxiong glucose injection, strengthen ginseng rhizome of chuanxiong glucose injection agent security detection management.
Embodiment
Can be well understood to the present invention further by specific embodiments of the invention given below, but they not limitation of the invention.
Embodiment 1
Chromatographic condition: chromatographic column is gel chromatographic columns, column temperature 30 DEG C, mobile phase: 2mmol/L ammonium acetate, flow velocity is 0.6mL/min, evaporative light dispersion dispersion (drift tube temperature 45 DEG C, dry gas flow velocity 0.2L/min), sample size: 5 μ L.
The preparation of standard solution:
Precision takes the dextran D4 reference substance 20mg being dried to constant weight at 80 DEG C, accurately weighed, puts in 5ml measuring bottle, adds water and make dissolving in right amount and be diluted to scale, shake up, and obtains every 1mL containing dextran D4 reference substance 4mg.
The preparation of need testing solution:
Get the ginseng rhizome of chuanxiong glucose injection of three batches respectively, cross 0.45 μm of miillpore filter, obtain need testing solution.
Assay method:
Get standard solution and each 5 μ L of need testing solution respectively, detect through HPLC-ELSD.In test sample chromatogram, appearance time is greater than dextran D4 reference substance impurity peaks is large molecule, amasss percentage calculation be greater than dextran D4 reference substance impurity peaks sharp side and amass accounting by sharp side.
Testing result is in table 1
Table 1
| Lot number | Large molecule peak area | Total peak area | Peak area ratio shared by large molecule |
| 20150207 | 32.1 | 73131.5 | 0.04 |
| 20150208 | 28.8 | 72555.9 | 0.04 |
| 20150209 | 28.1 | 72745.2 | 0.04 |
Embodiment 2
Chromatographic condition: chromatographic column is gel chromatographic columns, column temperature 35 DEG C, mobile phase: 4mmol/L ammonium acetate, flow velocity is 0.8mL/min, evaporative light dispersion dispersion (drift tube temperature 48 DEG C, dry gas flow velocity 0.5L/min), sample size: 5 μ L.
The preparation of standard solution:
Precision takes the dextran D4 reference substance 20mg being dried to constant weight at 80 DEG C, accurately weighed, puts in 5ml measuring bottle, adds water and make dissolving in right amount and be diluted to scale, shake up, and obtains every 1mL containing dextran D4 reference substance 4mg.
The preparation of need testing solution:
Get the ginseng rhizome of chuanxiong glucose injection of three batches respectively, cross 0.45 μm of miillpore filter, obtain need testing solution.
Assay method:
Get standard solution and each 5 μ L of need testing solution respectively, detect through HPLC-ELSD.In test sample chromatogram, appearance time is greater than dextran D4 reference substance impurity peaks is large molecule, amasss percentage calculation be greater than dextran D4 reference substance impurity peaks sharp side and amass accounting by sharp side.
Testing result is in table 2
Table 2
| Lot number | Large molecule peak area | Total peak area | Peak area ratio shared by large molecule |
| 20150207 | 32.3 | 73135.5 | 0.04 |
| 20150208 | 28.7 | 72558.4 | 0.04 |
| 20150209 | 28.3 | 72747.0 | 0.04 |
Embodiment 3
Chromatographic condition: chromatographic column is gel chromatographic columns, column temperature 40 DEG C, mobile phase: 5mmol/L ammonium acetate, flow velocity is 0.8mL/min, evaporative light dispersion dispersion (drift tube temperature 48 DEG C, dry gas flow velocity 0.5L/min), sample size: 5 μ L.
The preparation of standard solution:
Precision takes the dextran D4 reference substance 20mg being dried to constant weight at 80 DEG C, accurately weighed, puts in 5ml measuring bottle, adds water and make dissolving in right amount and be diluted to scale, shake up, and obtains every 1mL containing dextran D4 reference substance 4mg.
The preparation of need testing solution:
Get the ginseng rhizome of chuanxiong glucose injection of three batches respectively, cross 0.45 μm of miillpore filter, obtain need testing solution.
Assay method:
Get standard solution and each 5 μ L of need testing solution respectively, detect through HPLC-ELSD.In test sample chromatogram, appearance time is greater than dextran D4 reference substance impurity peaks is large molecule, amasss percentage calculation be greater than dextran D4 reference substance impurity peaks sharp side and amass accounting by sharp side.
Testing result is in table 3
Table 3
| Lot number | Large molecule peak area | Total peak area | Peak area ratio shared by large molecule |
| 20150207 | 31.7 | 73146.4 | 0.04 |
| 20150208 | 27.6 | 72554.2 | 0.04 |
| 20150209 | 26.9 | 72753.1 | 0.04 |
Embodiment 4
Chromatographic condition: chromatographic column is gel chromatographic columns, column temperature 45 DEG C, mobile phase: 6mmol/L ammonium acetate, flow velocity is 1.2mL/min, evaporative light dispersion dispersion (drift tube temperature 55 DEG C, dry gas flow velocity 1.0L/min), sample size: 5 μ L.
The preparation of standard solution:
Precision takes the dextran D4 reference substance 20mg being dried to constant weight at 80 DEG C, accurately weighed, puts in 5ml measuring bottle, adds water and make dissolving in right amount and be diluted to scale, shake up, and obtains every 1mL containing dextran D4 reference substance 4mg.
The preparation of need testing solution:
Get the ginseng rhizome of chuanxiong glucose injection of three batches respectively, cross 0.45 μm of miillpore filter, obtain need testing solution.
Assay method:
Get standard solution and each 5 μ L of need testing solution respectively, detect through HPLC-ELSD.In test sample chromatogram, appearance time is greater than dextran D4 reference substance impurity peaks is large molecule, amasss percentage calculation be greater than dextran D4 reference substance impurity peaks sharp side and amass accounting by sharp side.
Testing result is in table 4
Table 4
| Lot number | Large molecule peak area | Total peak area | Peak area ratio shared by large molecule |
| 20150207 | 30.3 | 73137.1 | 0.04 |
| 20150208 | 26.8 | 72561.7 | 0.04 |
| 20150209 | 27.3 | 72746.9 | 0.04 |
According to above-mentioned analysis of experimental data, the present invention can detect macromolecular content in ginseng rhizome of chuanxiong glucose injection effectively, and sample repeatability is good, and accuracy is high, and more can ensure accuracy, the validity of testing result.
Claims (1)
1. join macromolecular substances detection method in rhizome of chuanxiong glucose injection, it is characterized in that, be made up of following steps:
(1) following chromatographic condition is set up:
Chromatographic condition: gel chromatographic columns, column temperature 25 ~ 50 DEG C, mobile phase: 1 ~ 7mmol/L ammonium acetate, flow velocity is 0.5 ~ 1.5mL/min, the drift tube temperature 40 ~ 60 DEG C of setting evaporative light dispersion dispersion, dry gas flow velocity 0.2 ~ 1.2L/min, sample size: 5 μ L;
(2) preparation of standard solution:
Precision takes the dextran D4 reference substance 20mg being dried to constant weight at 80 DEG C, accurately weighed, puts in 5ml measuring bottle, adds water and make dissolving in right amount and be diluted to scale, shake up, and obtains every 1mL containing dextran D4 reference substance 4mg;
(3) preparation of need testing solution:
Get the ginseng rhizome of chuanxiong glucose injection of different lot number respectively, cross 0.45 μm of miillpore filter, obtain need testing solution;
(4) measure:
Get standard solution prepared by step (2) and each 5 μ L of need testing solution prepared by step (3) respectively, detect through HPLC-ELSD; In test sample chromatogram, appearance time is greater than dextran D4 reference substance impurity peaks is large molecule, amasss percentage calculation be greater than dextran D4 reference substance impurity peaks sharp side and amass accounting by sharp side.
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| CN201510973210.3A CN105467035A (en) | 2015-12-22 | 2015-12-22 | Method for detecting macromolecular substances in Shenxiong glucose injection |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107340344A (en) * | 2017-07-18 | 2017-11-10 | 黑龙江珍宝岛药业股份有限公司 | The detection method of macromolecular substances in a kind of Shu Xuening injection |
| CN109324133A (en) * | 2018-11-02 | 2019-02-12 | 华润三九（雅安）药业有限公司 | The detection method of polymer substance in traditional Chinese medicine injection |
| CN109709241A (en) * | 2019-01-30 | 2019-05-03 | 浙江大学 | The measuring method of high molecular weight substance in Chinese medicine injection containing liposoluble ingredient |
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| JP2006194724A (en) * | 2005-01-13 | 2006-07-27 | Toray Ind Inc | Separation membrane for protein and/or peptide analysis pretreatment |
| CN102445500A (en) * | 2010-10-14 | 2012-05-09 | 天津天士力之骄药业有限公司 | Method for detecting macromolecular substances in Yiqifumai injection |
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2015
- 2015-12-22 CN CN201510973210.3A patent/CN105467035A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2006194724A (en) * | 2005-01-13 | 2006-07-27 | Toray Ind Inc | Separation membrane for protein and/or peptide analysis pretreatment |
| CN102445500A (en) * | 2010-10-14 | 2012-05-09 | 天津天士力之骄药业有限公司 | Method for detecting macromolecular substances in Yiqifumai injection |
Non-Patent Citations (5)
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| 吕 兰等: "1. 参芎葡萄糖注射液中大分子物质检测方法，其特征在于，由以下步骤组成：", 《世界临床药物》 * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107340344A (en) * | 2017-07-18 | 2017-11-10 | 黑龙江珍宝岛药业股份有限公司 | The detection method of macromolecular substances in a kind of Shu Xuening injection |
| CN109324133A (en) * | 2018-11-02 | 2019-02-12 | 华润三九（雅安）药业有限公司 | The detection method of polymer substance in traditional Chinese medicine injection |
| CN109324133B (en) * | 2018-11-02 | 2021-09-07 | 华润三九（雅安）药业有限公司 | Method for detecting high molecular substance in Chinese medicine injection |
| CN109709241A (en) * | 2019-01-30 | 2019-05-03 | 浙江大学 | The measuring method of high molecular weight substance in Chinese medicine injection containing liposoluble ingredient |
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