CN106525819A - Method for measuring content of magnesium salt in icodextrin bulk drug - Google Patents
Method for measuring content of magnesium salt in icodextrin bulk drug Download PDFInfo
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- CN106525819A CN106525819A CN201510570543.1A CN201510570543A CN106525819A CN 106525819 A CN106525819 A CN 106525819A CN 201510570543 A CN201510570543 A CN 201510570543A CN 106525819 A CN106525819 A CN 106525819A
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- icodextrin
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Abstract
The invention belongs to the field of medical technology and relates to a method for measuring content of magnesium salt in icodextrin bulk drug. The method comprises the following steps: accurately weighing 0.1 g of icodextrin bulk drug, carrying out microwave digestion, transferring a sample solution into a 100ml PET volumetric flask, and keeping a constant volume by the use of water; preparing standard solutions with magnesium concentrations respectively being 0 ug/ml, 0.05 ug/ml, 0.1 ug/ml, 0.5 ug/ml, 1 ug/ml and 3 ug/ml; successively measuring strengths of the standard solutions and the sample solution under the condition of set inductively coupled plasma emission spectrometer parameters, drawing a calibration curve according to the strengths of the standard solutions, and comparing the calibration curve with a standard curve to obtain content of magnesium salt in the icodextrin bulk drug. The measurement method has high sensitivity and good repeatability, and realizes accurate measurement of magnesium salt in the icodextrin bulk drug. The method is simple to operate, is beneficial to reduce test cost and helps enhance product quality and safety.
Description
Technical field
The invention belongs to pharmaceutical technology field, specifically, is related to a kind of assay method of magnesium salt content in icodextrin crude drug.
Background technology
Peritoneal dialysis solution is to ensure one of important element that peritoneal dialysis are smoothed out.So far, glucose dialysis are still to make
With most peritoneal dialysis solutions, it is currently unique dialysis solution in China.With the raising of dialysis, clinically continuously emerge
Novel dialytic liquid, the icodextrin dialysis solution with polyglucose as penetrating agent are exactly one kind therein.In icodextrin crude drug
The presence of Mg salt directly affects the quality of icodextrin peritoneal dialysis solution, therefore is to need to grind in research process to the control of Mg salt
One of important content studied carefully.Determine at present Mg salt contents method mainly have atomic absorption spectrophotometry (flame atomization,
Sampling Graphite Furnace Atomic method), but atomic absorption spectrophotometry has that precision is poor, sensitivity is low, poor repeatability.
The content of the invention
It is an object of the invention to overcome prior art to there is shortcoming, seek design a kind of based on inductively coupled plasma launching light
In a kind of icodextrin crude drug of spectrum (ICP-OES) method, the assay method of magnesium salt content, realizes magnesium salt in icodextrin crude drug
Accurate measure, sensitivity is high, reproducible, while meeting the indices of check item Method validation.
To achieve these goals, the technical solution used in the present invention is：The measure of magnesium salt content in a kind of icodextrin crude drug
Method, comprises the following steps：
Step 1：Sample pretreatment
0.1g icodextrin crude drug is accurately weighed, is added in micro-wave diminishing pot, addition 5ml water and 8ml mass percents are
65% nitric acid, closes the lid after shaking up placement several minutes；
Step 2：Micro-wave digestion
According to following parameter setting microwave dissolver：200 DEG C of design temperature, intensification 25min are incubated 20min；After the completion of clearing up
Automatically lower the temperature, take out micro-wave diminishing pot, open lid, sample solution is transferred to into 100mlPET after nitrogen dioxide gas are evaporated completely
In volumetric flask, water constant volume is used；
Step 3：Preparing standard solution
Precision measures the magnesium single element standard solution 1ml that magnesium density is 1000ug/ml, is placed in 200ml measuring bottles, dilute
To scale, shake up and obtain final product magnesium single element contrast solution, the 5 μ g containing magnesium in every 1ml；Precision measure magnesium single element contrast solution 0ml,
In 1ml, 2ml, 10ml, 20ml, 60ml to 100mlPET volumetric flasks, constant volume, obtain final product magnesium density be respectively 0ug/ml, 0.05
The standard solution of ug/ml, 0.1ug/ml, 0.5ug/ml, 1ug/ml and 3ug/ml；
Step 4：Determine
In the inductive coupling plasma emission spectrograph parameter of setting：Power：1.2kw, plasma flow amount：10.00L/min,
Secondary air amount：0.60L/min, carrier gas：0.70L/min, sample introduction speed：Under the conditions of 1.5mL/min, measurement standard successively
The intensity of solution and sample solution, draws calibration curve according to the intensity of standard solution, obtains Chinese mugwort to be measured with standard curve contrast and examines
Magnesium salt content in dextrin crude drug.
Following checking has been carried out to the assay method of the present invention：
(1) the linear of this method, scope and test limit
Linear and scope such as following table：
With Mg salinity as vertical coordinate, absorbance is abscissa, and test obtains the linear relationship of Mg salinity and absorbance
Y=1.722x+0.000, R2=0.998, correlation coefficient is 0.9999；By data above it can be seen that in the range of the 0-3ug/ml this
The assay method of invention has good linear；
Imposing a condition：Power：1.2kw, plasma flow amount：10.00L/min, secondary air amount：0.60L/min,
Carrier gas：0.70L/min, sample introduction speed：Under the conditions of 1.5mL/min, 6 measure, the blank solution is carried out to blank solution
For 10% dilute nitric acid solution, its standard deviation is calculated, with 3 times of standard deviation as its detection limit, calculate the detection of each element
It is limited to 0.002ug/ml.
(2) response rate of assay method of the present invention
The response rate of 2 assay method of table
By data in table 2 it is known that the assay method of the present invention has good accuracy.
(3) precision of assay method of the present invention
The precision of 3 assay method of table
By the data in table 3 it is known that the assay method precision of the present invention is good.
Beneficial effects of the present invention are：The method of testing sensitivity of the present invention is high, reproducible, realizes to icodextrin raw material
The Accurate Determining of medicine magnesium salt；It is simple to operate, testing cost is advantageously reduced, while improve product quality and safety.
Specific embodiment
Below by specific embodiment, the invention will be further described：
Embodiment 1：
In the icodextrin crude drug of the present embodiment, the assay method of magnesium salt content, comprises the following steps：
Step 1：Sample pretreatment
0.1g icodextrin crude drug is accurately weighed, is added in micro-wave diminishing pot, addition 5ml water and 8ml mass percents are
65% nitric acid, closes the lid after shaking up placement several minutes；
Step 2：Micro-wave digestion
According to following parameter setting microwave dissolver：200 DEG C of design temperature, intensification 25min are incubated 20min；After the completion of clearing up
Automatically lower the temperature, take out micro-wave diminishing pot, open lid, sample solution is transferred to into 100mlPET after nitrogen dioxide gas are evaporated completely
In volumetric flask, water constant volume is used；
Step 3：Preparing standard solution
Precision measures the magnesium single element standard solution 1ml that concentration is 1000ug/ml, is placed in 200ml measuring bottles, is diluted with water to
Scale, shakes up and obtains final product magnesium single element contrast solution, the 5 μ g containing magnesium in every 1ml；Precision measure magnesium single element contrast solution 0ml, 1ml,
In 2ml, 10ml, 20ml, 60ml to 100mlPET volumetric flasks, constant volume, obtain final product magnesium density be respectively 0ug/ml, 0.05ug/ml,
The standard solution of 0.1ug/ml, 0.5ug/ml, 1ug/ml and 3ug/ml；
Step 4：Determine
In the inductive coupling plasma emission spectrograph parameter selected：Power：1.2kw, plasma flow amount：10.00L/min,
Secondary air amount：0.60L/min, carrier gas：0.70L/min, sample introduction speed：Under the conditions of 1.5mL/min, measurement standard successively
The intensity of solution and sample solution, draws calibration curve according to the intensity of standard solution, obtains Chinese mugwort to be measured with standard curve contrast and examines
Magnesium salt content in dextrin crude drug.
Claims (1)
1. in a kind of icodextrin crude drug magnesium salt content assay method, it is characterised in that comprise the following steps：
Step 1：Sample pretreatment
0.1g icodextrin crude drug is accurately weighed, is added in micro-wave diminishing pot, addition 5ml water and 8ml mass percents are
65% nitric acid, closes the lid after shaking up placement several minutes；
Step 2：Micro-wave digestion
According to following parameter setting microwave dissolver：200 DEG C of design temperature, intensification 25min are incubated 20min；After the completion of clearing up
Automatically lower the temperature, take out micro-wave diminishing pot, open lid, sample solution is transferred to into 100mlPET after nitrogen dioxide gas are evaporated completely
In volumetric flask, water constant volume is used；
Step 3：Preparing standard solution
Precision measures the magnesium single element standard solution 1ml that magnesium density is 1000ug/ml, is placed in 200ml measuring bottles, dilute
To scale, shake up and obtain final product magnesium single element contrast solution, the 5 μ g containing magnesium in every 1ml；Precision measure magnesium single element contrast solution 0ml,
In 1ml, 2ml, 10ml, 20ml, 60ml to 100mlPET volumetric flasks, constant volume, obtain final product magnesium density be respectively 0ug/ml, 0.05
The standard solution of ug/ml, 0.1ug/ml, 0.5ug/ml, 1ug/ml and 3ug/ml；
Step 4：Determine
In the inductive coupling plasma emission spectrograph parameter of setting：Power：1.2kw, plasma flow amount：10.00L/min,
Secondary air amount：0.60L/min, carrier gas：0.70L/min, sample introduction speed：Under the conditions of 1.5mL/min, measurement standard successively
The intensity of solution and sample solution, draws calibration curve according to the intensity of standard solution, obtains Chinese mugwort to be measured with standard curve contrast and examines
Magnesium salt content in dextrin crude drug.
Priority Applications (1)
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| CN201510570543.1A CN106525819A (en) | 2015-09-09 | 2015-09-09 | Method for measuring content of magnesium salt in icodextrin bulk drug |
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| CN201510570543.1A CN106525819A (en) | 2015-09-09 | 2015-09-09 | Method for measuring content of magnesium salt in icodextrin bulk drug |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN117050201A (en) * | 2023-07-31 | 2023-11-14 | 武汉华科大生命科技有限公司 | Method for removing aluminum salt and magnesium salt in icodextrin bulk drug |
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| CN1778958A (en) * | 2004-11-23 | 2006-05-31 | 苏州艾杰生物科技有限公司 | Determination of magnesium ion content from enzyme method and magnesium ion diagnostic reagent kit |
| CN103901018A (en) * | 2014-03-14 | 2014-07-02 | 广西出入境检验检疫局危险品检测技术中心 | Measurement method for content of magnesium and content of aluminium in main component of pyrotechnic composition for fireworks and crackers |
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2015
- 2015-09-09 CN CN201510570543.1A patent/CN106525819A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1778958A (en) * | 2004-11-23 | 2006-05-31 | 苏州艾杰生物科技有限公司 | Determination of magnesium ion content from enzyme method and magnesium ion diagnostic reagent kit |
| CN103901018A (en) * | 2014-03-14 | 2014-07-02 | 广西出入境检验检疫局危险品检测技术中心 | Measurement method for content of magnesium and content of aluminium in main component of pyrotechnic composition for fireworks and crackers |
Non-Patent Citations (3)
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| 萨嘎拉: "高压密封微波消解-等离子体发射光谱法测定5种蒙药中镁、钙、锰、铁、钴、镍、铜和锶", 《光谱实验室》 * |
| 谢绍金 等: "ICP-AES测定2E12铝合金中钛、铜、镁、锰、锌、铬、硅和铁的研究", 《分析仪器》 * |
| 陈阳: "电感耦合等离子体原子发射光谱法和原子吸收光谱法在药品质量控制中的应用", 《中国硕士学位论文全文数据库》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN117050201A (en) * | 2023-07-31 | 2023-11-14 | 武汉华科大生命科技有限公司 | Method for removing aluminum salt and magnesium salt in icodextrin bulk drug |
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Application publication date: 20170322 |