CN104792902A - Method for detecting sodium chloride content in sodium chloride injection - Google Patents
Method for detecting sodium chloride content in sodium chloride injection Download PDFInfo
- Publication number
- CN104792902A CN104792902A CN201510238978.6A CN201510238978A CN104792902A CN 104792902 A CN104792902 A CN 104792902A CN 201510238978 A CN201510238978 A CN 201510238978A CN 104792902 A CN104792902 A CN 104792902A
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- China
- Prior art keywords
- sodium chloride
- high performance
- performance liquid
- water
- alcohol
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Links
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 title claims abstract description 32
- 239000011780 sodium chloride Substances 0.000 title claims abstract description 16
- 239000008354 sodium chloride injection Substances 0.000 title claims abstract description 13
- 238000000034 method Methods 0.000 title abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000004128 high performance liquid chromatography Methods 0.000 claims abstract description 8
- 239000007921 spray Substances 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 11
- 238000003556 assay Methods 0.000 claims description 8
- 239000011159 matrix material Substances 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 3
- 238000001514 detection method Methods 0.000 abstract description 3
- 235000019441 ethanol Nutrition 0.000 abstract 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical group O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 9
- 238000012360 testing method Methods 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 239000012491 analyte Substances 0.000 description 2
- 238000010828 elution Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000003182 parenteral nutrition solution Substances 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
Landscapes
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention discloses a method for detecting sodium chloride content in sodium chloride injection. The method comprises the following steps: 1, sample pretreatment, namely dissolving 50mg of a sample by 35ml of water, fixing the volume to be constant to 100ml by ethyl alcohol; and 2, analyzing by high performance liquid chromatography, wherein the parameters of the high performance liquid chromatography are set as follows: the flowing phase is ethyl alcohol-water, the flow rate is 1ml/min, and the column temperature is 45 degree centigrade. The invention aims to provides the method for detecting sodium chloride content in sodium chloride injection which is accuracy in detection and easy to operate.
Description
Technical field
The present invention relates to detection field, particularly the assay method of sodium chloride content in a kind of sodium chloride injection.
Background technology
Chinese Pharmacopoeia 2010 editions describes sodium chloride method for measuring in sodium chloride injection, its 3.6.2 saves record and adopts silver nitrate titration method to measure the content of the sodium chloride in parenteral solution, the method requires high to operating personnel's professional skill, and different tester's test result exists certain deviation.
Summary of the invention
The object of the present invention is to provide a kind of assay method measuring sodium chloride content in sodium chloride injection accurate, simple to operate.
Technical scheme of the present invention is: the assay method of sodium chloride content in a kind of sodium chloride injection, comprises the following steps:
Step 1: sample pretreatment, is settled to 100ml with ethanol after the water-soluble solution of sample thief 50mg 35ml;
Step 2: adopt high performance liquid chromatography to analyze;
The optimum configurations that high performance liquid chromatography carries out analyzing is as follows:
Mobile phase: alcohol-water; Flow velocity: 1ml/min; Column temperature: 45 DEG C;
Chromatographic column: Thermo Acclaim mixed-matrix chromatographic column, 4.6 μm × 250mm, 5 μm; In described mobile phase, the volume ratio of second alcohol and water is 60:40 ~ 70:30; The volume ratio of described mobile phase second alcohol and water in 0 minute to 7 minutes sections rises to 70:30 by 60:40 uniformly; Then in 7 minutes to 25 minutes sections, the volume ratio of second alcohol and water is constant in 70:30;
The model of described high performance liquid chromatograph is: hermo U3000 high performance liquid chromatograph, the subsidiary Corona Ultra electron spray detecting device of described hermo U3000 high performance liquid chromatograph, described Corona Ultra electron spray detecting device is used for the solute transfer charge of the Thermo Acclaim mixed-matrix chromatographic column mobile phase out of high performance liquid chromatograph, and by the gatherer of Corona Ultra electron spray detecting device detect solute the electrically charged concentration determining solute.
In above-mentioned sodium chloride injection sodium chloride content assay method in, described Corona Ultra electron spray detecting device is connected with the outlet of Thermo Acclaim mixed-matrix chromatographic column.
Beneficial effect of the present invention is as follows:
Method of testing of the present invention adopts the mode of gradient elution to carry out wash-out, sodium chloride generally can wash-out before 7 minutes, therefore ladder wash-out 7 minutes afterchlorinate sodium substantially can wash-out, and be eluted to 25 minutes, ensure that chromatographic column can wash-out completely, column temperature, a little more than room temperature, can avoid assorted peak to disturb; Can realize effective separation of composition to be measured in wider scope, meanwhile, employing Corona Ultra electron spray detecting device can realize Measurement accuracy during extremely low concentration, the instability that the manual operation overcoming conventional test methodologies brings.
Adopt such scheme can the measuring accuracy of sodium chloride effectively in sodium chloride injection, avoid the error of manual operation generation.
Embodiment
Below in conjunction with embodiment, technical scheme of the present invention is described in further detail, but does not form any limitation of the invention.
Embodiment 1
An assay method for sodium chloride content in sodium chloride injection, comprises the following steps:
Step 1: sample pretreatment, is settled to 100ml with ethanol after the water-soluble solution of sample thief 50mg 35ml;
Step 2: adopt high performance liquid chromatography to analyze;
The optimum configurations that high performance liquid chromatography carries out analyzing is as follows:
Mobile phase: alcohol-water; Flow velocity: 1ml/min; Column temperature: 45 DEG C;
Chromatographic column: Thermo Acclaim mixed-matrix chromatographic column, 4.6 μm × 250mm, 5 μm; In described mobile phase, the volume ratio of second alcohol and water is 60:40 ~ 70:30; The volume ratio of described mobile phase second alcohol and water in 0 minute to 7 minutes sections rises to 70:30 by 60:40 uniformly; Then in 7 minutes to 25 minutes sections, the volume ratio of second alcohol and water is constant in 70:30;
The model of described high performance liquid chromatograph is: hermo U3000 high performance liquid chromatograph, the subsidiary Corona Ultra electron spray detecting device of described hermo U3000 high performance liquid chromatograph, described Corona Ultra electron spray detecting device is connected with the outlet of Thermo Acclaim mixed-matrix chromatographic column.The principle of work of Corona Ultra electron spray detecting device (CAD) technology is that analysis thing is changed into particles of solute.The size of particle increases along with the content of analyte; Particles of solute and positively charged nitrogen particle bump against, and electric charge transfers to (particles of solute is larger, charged more) on particle thereupon; Particles of solute to gatherer, measures the carried charge of particles of solute their Charger transfer by highly sensitive electrostatic detection, consequent marking current is directly proportional to the content of solute.Testing result is relevant with analyte particles, and marking current is directly proportional to the quality analyzing thing in sample.
Above-mentioned method of testing adopts the mode of gradient elution to carry out wash-out, and sodium chloride generally can wash-out before 7 minutes, and therefore ladder wash-out 7 minutes afterchlorinate sodium substantially can wash-out, and be eluted to 25 minutes, ensure that chromatographic column can wash-out completely, column temperature, a little more than room temperature, can avoid assorted peak to disturb; Can realize effective separation of composition to be measured in wider scope, meanwhile, employing Corona Ultra electron spray detecting device can realize Measurement accuracy during extremely low concentration, the instability that the manual operation overcoming conventional test methodologies brings.
Above-describedly be only preferred embodiment of the present invention, all do within the scope of the spirit and principles in the present invention any amendment, equivalently to replace and improvement etc., all should be included within protection scope of the present invention.
Claims (2)
1. the assay method of sodium chloride content in sodium chloride injection, is characterized in that, comprise the following steps:
Step 1: sample pretreatment, is settled to 100ml with ethanol after the water-soluble solution of sample thief 50mg 35ml;
Step 2: adopt high performance liquid chromatography to analyze;
The optimum configurations that high performance liquid chromatography carries out analyzing is as follows:
Mobile phase: alcohol-water; Flow velocity: 1ml/min; Column temperature: 45 DEG C;
Chromatographic column: Thermo Acclaim mixed-matrix chromatographic column, 4.6 μm × 250mm, 5 μm; In described mobile phase, the volume ratio of second alcohol and water is 60:40 ~ 70:30; The volume ratio of described mobile phase second alcohol and water in 0 minute to 7 minutes sections rises to 70:30 by 60:40 uniformly; Then in 7 minutes to 25 minutes sections, the volume ratio of second alcohol and water is constant in 70:30;
The model of described high performance liquid chromatograph is: hermo U3000 high performance liquid chromatograph, the subsidiary Corona Ultra electron spray detecting device of described hermo U3000 high performance liquid chromatograph, described Corona Ultra electron spray detecting device is used for the solute transfer charge of the Thermo Acclaim mixed-matrix chromatographic column mobile phase out of high performance liquid chromatograph, and by the gatherer of Corona Ultra electron spray detecting device detect solute the electrically charged concentration determining solute.
2. the assay method of sodium chloride content in sodium chloride injection according to claim 1, it is characterized in that, described Corona Ultra electron spray detecting device is connected with the outlet of Thermo Acclaim mixed-matrix chromatographic column.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510238978.6A CN104792902B (en) | 2015-05-12 | 2015-05-12 | The assay method of sodium chloride content in a kind of sodium chloride injection |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510238978.6A CN104792902B (en) | 2015-05-12 | 2015-05-12 | The assay method of sodium chloride content in a kind of sodium chloride injection |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104792902A true CN104792902A (en) | 2015-07-22 |
| CN104792902B CN104792902B (en) | 2016-06-29 |
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| CN201510238978.6A Active CN104792902B (en) | 2015-05-12 | 2015-05-12 | The assay method of sodium chloride content in a kind of sodium chloride injection |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009124294A2 (en) * | 2008-04-05 | 2009-10-08 | Lpath, Inc. | Pharmaceutical compositions for binding sphingosine-1-phosphate |
| 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 |
-
2015
- 2015-05-12 CN CN201510238978.6A patent/CN104792902B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009124294A2 (en) * | 2008-04-05 | 2009-10-08 | Lpath, Inc. | Pharmaceutical compositions for binding sphingosine-1-phosphate |
| 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 (4)
| Title |
|---|
| CHRISTOPHER CRAFTS等: "Evaluation of Methods for the Simultaneous Analysis of Cations and Anions Using HPLC with Charged Aerosol Detection and a Zwitterionic Stationary Phase", 《JOURNAL OF CHROMATOGRAPHIC SCIENCE》 * |
| KE ZHANG等: "Simultaneous determination of positive and negative pharmaceutical counterions using mixed-mode chromatography coupled with charged aerosol detector", 《JOURNAL OF CHROMATOGRAPHY A》 * |
| Z.HUANG等: "Determination of inorganic pharmaceutical counterions using hydrophilic interaction chromatography coupled with a Corona CAD detector", 《JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS》 * |
| 刘立洋等: "一种新型的通用型检测器——电喷雾检测器", 《现代科学仪器》 * |
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| CN104792902B (en) | 2016-06-29 |
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Effective date of registration: 20180105 Address after: 543000 the Guangxi Zhuang Autonomous Region Cenxi North Road No. 5 Patentee after: Cenxi Productivity Promotion Center Address before: 543000 the Guangxi Zhuang Autonomous Region, Wuzhou West Ring Road, No. 198 Patentee before: WUZHOU INSTITUTE FOR FOOD AND DRUG CONTROL, GUANGXI ZHUANG AUTONOMOUS REGION |
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| CB03 | Change of inventor or designer information |
Inventor after: Sun Liangguang Inventor after: Guo Zhenwang Inventor after: Chen Xuesong Inventor after: Lai Xiumei Inventor after: Huang Heng Inventor after: Li Zhirui Inventor after: Zhang Yunping Inventor before: Chen Xuesong Inventor before: Lai Xiumei Inventor before: Huang Heng Inventor before: Li Zhirui Inventor before: Zhang Yunping |
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Effective date of registration: 20180426 Address after: 543000 198 West Ring Road, Wuzhou, the Guangxi Zhuang Autonomous Region Patentee after: WUZHOU FOOD AND DRUG INSPECTION INSTITUTE Address before: No. 5 north mountain road, Cenxi, the Guangxi Zhuang Autonomous Region Patentee before: Cenxi Productivity Promotion Center |
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Application publication date: 20150722 Assignee: GUANGXI GUILIN RUIDE DETECTION AUTHENTICATION TECHNOLOGY Co.,Ltd. Assignor: WUZHOU FOOD AND DRUG INSPECTION INSTITUTE Contract record no.: X2022450000291 Denomination of invention: A method for determination of sodium chloride content in sodium chloride injection Granted publication date: 20160629 License type: Common License Record date: 20221214 |
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