CN105203650A - Method for detecting content of glucose in peritoneal dialysis solution - Google Patents
Method for detecting content of glucose in peritoneal dialysis solution Download PDFInfo
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- CN105203650A CN105203650A CN201410298138.4A CN201410298138A CN105203650A CN 105203650 A CN105203650 A CN 105203650A CN 201410298138 A CN201410298138 A CN 201410298138A CN 105203650 A CN105203650 A CN 105203650A
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Abstract
The invention relates to a method for detecting the content of glucose in a peritoneal dialysis solution. The method comprises the following steps: precisely weighing an anhydrous glucose reference substance, and dissolving and diluting through deionized water so as to obtain a solution, wherein 1 ml of the solution contains 5.0-6.5 mg of glucose; precisely weighing a neutral peritoneal dialysis solution and diluting through deionized water so as to obtain another solution, wherein 1 ml of the solution contains 5.0-6.5 mg of glucose; respectively and precisely taking 20 [mu]l of a reference solution and a test solution, injecting the reference solution and the test solution into a chromatographic instrument, recording a chromatogram, and calculating as a peak area according to an external standard method so as to obtain labelled amount of glucose, wherein chromatographic conditions are as follows: the chromatographic column is a WatersSugarParkI column, 300 mm*6.5 mm, 6.5 [mu] m; a mobile phase is deionized water; the flow velocity is 0.5+/-0.1 ml/min; the column temperature is 80+/-5 DEG C; the set temperature of a refractive index detector is 40+/-5 DEG C and the sample amount is 20 [mu]l. According to the invention, the content of glucose in the peritoneal dialysis solution is detected through the high performance liquid chromatography, the quality of the peritoneal dialysis solution is controlled precisely, the process optimization is facilitated and the product quality and safety are improved.
Description
Technical field
The present invention relates to medical art, specifically the detection method of glucose content in a kind of peritoneal dialysis solution.
Background technology
In peritoneal dialysis solution (lactate) state quality standard draft, have employed indirect iodometric processes and back titration method measures glucose content.Concrete grammar is: it is appropriate that precision measures this product, precision adds iodine titration solution (0.1mol/L) 25ml, jolting limit, limit drips sodium hydroxide titration liquid (0.1mol/L) 50ml, shake up, in the dark place 30 minutes, add dilute sulfuric acid 5ml, with sodium thiosulfate vs (0.1mol/L) titration, during to nearly terminal, add starch indicator solution 2ml, continue to be titrated to blue disappearance, and the result blank test of titration is corrected, obtain, the iodine titration solution (0.1mol/L) of every 1ml is equivalent to the C of 9.909mg
6h
12o
6h
2o.
The reaction conditions that the method relates to is many, as precision adds the iodine titration solution 25ml of 0.1mol/L, precision adds 0.1mol/L sodium hydroxide titration liquid 50ml, limit edged jolting (jolting speed is uniform and stable), water seal (sometimes finding not have water seal good), in the dark the requirement such as to place 30 minutes, all can affect accuracy and the collimation of measurement result.Wherein I
2in water, solubleness is very little, and volatile, easily sees that light decomposes, and iodide ion is easy to by the O in air
2oxidation.In addition, when dripping sodium hydroxide solution, drop rate is not easily too fast, otherwise IO
-to have little time with glucose response and disproportionation is IO
3-and I
-, thus cause glucose not to be fully oxidized.These conditions above-mentioned all can bring considerable influence to the mensuration of glucose content, produce comparatively big error, to such an extent as to when doing Method validation to the method, glucose recovery data are higher or on the low side, can not the content of glucose in accurate response sample.
Glucose also uses specific rotation method to measure content usually, but due to the sodium lactate containing tool optical activity in peritoneal dialysis solution prescription, specific rotation method measures glucose and there is interference.
Summary of the invention
Point out according to above-mentioned deficiency, the object of this invention is to provide a kind of detection method being applicable to glucose content in peritoneal dialysis solution, abandon the analysis by titration that reaction is complicated, can control the content of glucose in peritoneal dialysis solution better, instruct technical study, improve the quality of products.
For achieving the above object, technical scheme of the present invention is: the detection method of glucose content in a kind of peritoneal dialysis solution, and it comprises the following steps:
(1) prepare reference substance solution: precision takes anhydrous dextrose reference substance, with deionized water dissolving, dilution, makes the solution containing glucose 5.0-6.5mg in every 1ml;
(2) prepare need testing solution: precision measures neutral peritoneal dialysis solution, make the solution containing glucose 5.0-6.5mg in every 1ml with deionized water dilution;
(3) essence gets contrast liquid and each 20 μ l of test liquid respectively, injecting chromatograph, and record chromatogram, by external standard method with calculated by peak area, obtains the labelled amount of glucose.
Wherein, described chromatographic condition is chromatographic column: WatersSugarParkI post, 300mm × 6.5mm, 6.5um; Mobile phase: deionized water; Flow velocity: 0.5 ± 0.1ml/min; Column temperature: 80 ± 5 DEG C; Composition distribution set temperature: 40 ± 5 DEG C; Sample size: 20 μ l.
Preferably: described chromatographic condition is chromatographic column: WatersSugarParkI post, 300mm × 6.5mm, 6.5um; Mobile phase: deionized water; Flow velocity: 0.5ml/min; Column temperature: 80 DEG C; Composition distribution set temperature: 40 DEG C; Sample size: 20 μ l.
Preferably: in described mobile phase deionized water, add bacteriostatic agent sodium azide.
Beneficial effect of the present invention is: the present invention, by high performance liquid chromatography, detects the content of glucose in peritoneal dialysis solution, accurately controls, be conducive to Optimization Technology, improve the quality of products and security to the quality of peritoneal dialysis solution.
Embodiment
Below in conjunction with specific embodiment, the present invention will be further described.
A detection method for glucose content in peritoneal dialysis solution, it comprises the following steps:
(1) prepare reference substance solution: precision takes anhydrous dextrose reference substance, with deionized water dissolving, dilution, makes the solution containing glucose 5.0-6.5mg in every 1ml;
(2) prepare need testing solution: precision measures neutral peritoneal dialysis solution, make the solution containing glucose 5.0-6.5mg in every 1ml with deionized water dilution;
(3) essence gets contrast liquid and each 20 μ l of test liquid respectively, injecting chromatograph, and record chromatogram, by external standard method with calculated by peak area, obtains the labelled amount of glucose.
Wherein, described chromatographic condition is chromatographic column: WatersSugarParkI post, 300mm × 6.5mm, 6.5um; Mobile phase: deionized water; Flow velocity: 0.5 ± 0.1ml/min; Column temperature: 80 ± 5 DEG C; Composition distribution set temperature: 40 ± 5 DEG C; Sample size: 20 μ l.
Preferred chromatographic condition is chromatographic column: WatersSugarParkI post, 300mm × 6.5mm, 6.5um; Mobile phase: deionized water; Flow velocity: 0.5ml/min; Column temperature: 80 DEG C; Composition distribution set temperature: 40 DEG C; Sample size: 20 μ l.
In order to prevent long bacterium in mobile phase from affecting test findings, in mobile phase deionized water, add bacteriostatic agent sodium azide.
Test and carried out a series of conditional filtering for whether adding sodium azide in the temperature of the column temperature of chromatographic column, detecting device, flow velocity and mobile phase (water).
First, raised respectively under the condition of original 80 DEG C and reduce by 5 DEG C by the column temperature of chromatographic column and test, found that, column temperature is 80 DEG C time, and chromatographic condition is best.Column temperature Difference test the results are shown in Table 1.
Table 1 column temperature Difference test result
| Column temperature | 75℃ | 80℃ | 85℃ |
| Glucose and fructose degree of separation | 2.66 | 2.87 | 2.77 |
| Glucose post is imitated | 2569.0 | 3936.5 | 3173.4 |
| Glucose tailing factor | 1.152 | 1.126 | 1.138 |
The temperature of detecting device raised respectively under the condition of original 40 DEG C again and reduce by 5 DEG C, found that detector temperature is 40 DEG C time, chromatographic condition is best.Detector temperature Difference test the results are shown in Table 2.
Table 2 detector temperature Difference test result
| Detector temperature | 35℃ | 40℃ | 45℃ |
| Glucose and fructose degree of separation | 2.78 | 2.87 | 2.77 |
| Glucose post school | 3288.4 | 3936.5 | 3222.6 |
| Glucose tailing factor | 1.129 | 1.126 | 1.136 |
Again flow velocity raised under the condition of original 0.5ml/min 0.1ml/min respectively and reduce 0.1ml/mn, found that flow velocity is when 0.5ml/min, in degree of separation preferably situation relative to tailing factor, post school is best.Flow velocity difference testing result is in table 3.
Table 3 flow velocity difference testing result
| Flow velocity | 0.4ml/min | 0.5ml/min | 0.6ml/min |
| Glucose and fructose degree of separation | 2.93 | 2.87 | 2.66 |
| Glucose post school | 3543.9 | 3936.5 | 2987.4 |
| Glucose tailing factor | 1.093 | 1.126 | 1.124 |
Then, in mobile phase (water), add appropriate bacteriostatic agent sodium azide, find that peak shape remains unchanged substantially in process of the test, sees all the time very well.When not adding sodium azide, test period one is long (because the saturating specification of this abdomen is many, batch larger, test period is long), peak shape just there will be change, more ugly, this is due to bacterium long in water, can only to stop test, pillar is unloaded down, because pillar can not organic solvent exposure, so adopt methyl alcohol or acetonitrile that system is rinsed about 60 minutes, with freshly prepd high purity water, the organic solvent in system is washed down, connect pillar and continue test, peak shape will be normal again.Such test is not only time-consuming but also require great effort.In process of the test after Xiang Shuizhong adds appropriate sodium azide or other bacteriostatic agents, peak shape is always fine, has both made test carry out very well, and has in turn saved the time.
One, high-efficient liquid phase technique accuracy validation
Precision takes each 3 parts totally 9 parts of 80%, 100%, 120% anhydrous dextrose of 1.36g (or 2.27g, 3.86g), put in 100ml measuring bottle respectively, add following solution respectively and (get anhydrous chlorides of rase sodium 5.44g, lime chloride 0.183g (or 0.257g), magnesium chloride 0.0508g, sodium lactate 4.48g respectively, be placed in 100ml measuring bottle, be dissolved in water, be diluted to scale, shake up, both.) 10ml, be diluted to scale by water-soluble solution, shake up; Precision measures above-mentioned solution 10ml, 6ml, 4ml respectively, in 25ml measuring bottle, is diluted with water to scale, shakes up, and makes the solution being about 5.5mg in every 1ml containing glucose, as need testing solution.Precision measures 20 μ l respectively, injection liquid chromatography, record chromatogram.Calculate the relative standard deviation of the recovery and the recovery, the result recovery should between 98.0% ~ 102.0%, RSD≤2.0%.Containing 1.5%, 2.5%, 4.25% glucose accuracy test result respectively in table 4,5,6.
Table 4 is containing 1.5% glucose accuracy test result
Table 5 is containing 2.5% glucose accuracy test result
Table 6 is containing 4.25% glucose accuracy test result
From table 4,5, the test findings of 6, adopt the inventive method to measure glucose content in peritoneal dialysis solution, its accuracy is good.
Two, high-efficient liquid phase technique precision checking
(1). repeatability: get this product, the need testing solution of preparation 6 parts of same concentrations, is tested according to above-mentioned glucose content detection method under condition identical as far as possible by an analyst, record glucose labelled amount.Containing 1.5%, 2.5%, 4.25% glucose preparation replica test result respectively in table 7,8,9.
Table 7 is containing 1.5% glucose preparation replica test result
Table 8 is containing 2.5% glucose preparation replica test result
Table 9 is containing 4.25% glucose preparation replica test result
From table 7,8, the test findings of 9, adopt the inventive method to measure glucose content in peritoneal dialysis solution, its repeatability is good.
(2). Intermediate precision: get this product, at different time by different analysts, parallel preparation 6 parts of test liquids, according to above-mentioned glucose content detection method, logging test results, calculates need testing solution content and relative standard deviation thereof.Containing 1.5% glucose preparation Intermediate precision test findings in table 10,11,12.
Table 10 is containing 1.5% glucose preparation Intermediate precision test findings
Table 11 is containing 2.5% glucose preparation Intermediate precision test findings
Table 12 is containing 4.25% glucose preparation Intermediate precision test findings
From table 10,11, the test findings of 12, adopt the inventive method to measure glucose content in peritoneal dialysis solution, its Intermediate precision is good.
Three, the recovery that records of titrimetry is in table 13.
Table 13 is containing 1.5% glucose accuracy test result
Table 4 is compared known with the test findings of table 13, adopts titrimetry to measure its accuracy of glucose content in peritoneal dialysis solution and comparatively adopt invention to measure the poor accuracy of glucose content in peritoneal dialysis solution.
Claims (3)
1. the detection method of glucose content in peritoneal dialysis solution, is characterized in that: it comprises the following steps:
(1) prepare reference substance solution: precision takes anhydrous dextrose reference substance, with deionized water dissolving, dilution, makes the solution containing glucose 5.0-6.5mg in every 1ml;
(2) prepare need testing solution: precision measures neutral peritoneal dialysis solution, make the solution containing glucose 5.0-6.5mg in every 1ml with deionized water dilution;
(3) essence gets contrast liquid and each 20 μ l of test liquid respectively, injecting chromatograph, and record chromatogram, by external standard method with calculated by peak area, obtains the labelled amount of glucose.
Wherein, described chromatographic condition is chromatographic column: WatersSugarParkI post, 300mm × 6.5mm, 6.5um; Mobile phase: deionized water; Flow velocity: 0.5 ± 0.1ml/min; Column temperature: 80 ± 5 DEG C; Composition distribution set temperature: 40 ± 5 DEG C; Sample size: 20 μ l.
2. the detection method of glucose content in peritoneal dialysis solution according to claim 1, is characterized in that: described chromatographic condition is chromatographic column: WatersSugarParkI post, 300mm × 6.5mm, 6.5um; Mobile phase: deionized water; Flow velocity: 0.5ml/min; Column temperature: 80 DEG C; Composition distribution set temperature: 40 DEG C; Sample size: 20 μ l.
3. the detection method of glucose content in peritoneal dialysis solution according to claim 1, is characterized in that: add bacteriostatic agent sodium azide in described mobile phase deionized water.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107561018A (en) * | 2016-06-30 | 2018-01-09 | 华仁药业股份有限公司 | A kind of method of glucose or glucose polymer content in measure compound preparation |
| CN109030656A (en) * | 2018-08-17 | 2018-12-18 | 华仁药业股份有限公司 | Detection method of the glucose in relation to substance in acetate Multiple electrolytes injection |
| CN109490236A (en) * | 2018-11-13 | 2019-03-19 | 华仁药业股份有限公司 | Impurity 3 in Icodextrin peritoneal dialysis solution, the detection method of 4-DGE |
| CN110308214A (en) * | 2019-04-26 | 2019-10-08 | 威高泰尔茂(威海)医疗制品有限公司 | The content assaying method of glucose converted product in neutral peritoneal dialysis solution |
| CN112180001A (en) * | 2020-08-22 | 2021-01-05 | 安徽丰原药业股份有限公司 | Method for detecting content of glucose in peritoneal dialysis solution |
| CN112505175A (en) * | 2020-11-20 | 2021-03-16 | 西安乐析医疗科技有限公司 | Method for determining content of impurities in peritoneal dialysis solution |
| CN114460202A (en) * | 2022-02-11 | 2022-05-10 | 山东威高肾科医疗器械有限公司 | Method for detecting concentration of glucose in hemodialysis solution |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107561018A (en) * | 2016-06-30 | 2018-01-09 | 华仁药业股份有限公司 | A kind of method of glucose or glucose polymer content in measure compound preparation |
| CN109030656A (en) * | 2018-08-17 | 2018-12-18 | 华仁药业股份有限公司 | Detection method of the glucose in relation to substance in acetate Multiple electrolytes injection |
| CN109490236A (en) * | 2018-11-13 | 2019-03-19 | 华仁药业股份有限公司 | Impurity 3 in Icodextrin peritoneal dialysis solution, the detection method of 4-DGE |
| CN110308214A (en) * | 2019-04-26 | 2019-10-08 | 威高泰尔茂(威海)医疗制品有限公司 | The content assaying method of glucose converted product in neutral peritoneal dialysis solution |
| CN112180001A (en) * | 2020-08-22 | 2021-01-05 | 安徽丰原药业股份有限公司 | Method for detecting content of glucose in peritoneal dialysis solution |
| CN112505175A (en) * | 2020-11-20 | 2021-03-16 | 西安乐析医疗科技有限公司 | Method for determining content of impurities in peritoneal dialysis solution |
| CN114460202A (en) * | 2022-02-11 | 2022-05-10 | 山东威高肾科医疗器械有限公司 | Method for detecting concentration of glucose in hemodialysis solution |
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Application publication date: 20151230 |