CN103175802A - Method for determining content of magnesium element in hydroxyethyl starch injection preparation - Google Patents

Method for determining content of magnesium element in hydroxyethyl starch injection preparation Download PDF

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CN103175802A
CN103175802A CN2011104293737A CN201110429373A CN103175802A CN 103175802 A CN103175802 A CN 103175802A CN 2011104293737 A CN2011104293737 A CN 2011104293737A CN 201110429373 A CN201110429373 A CN 201110429373A CN 103175802 A CN103175802 A CN 103175802A
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solution
magnesium
hydroxyethyl starch
single element
injection
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郁东梅
蔡作清
曹文俸
隗海瑞
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Sichuan Kelun Pharmaceutical Research Co Ltd
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Sichuan Kelun Pharmaceutical Research Co Ltd
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Abstract

The invention discloses a method for determining the content of a magnesium element in a hydroxyethyl starch injection preparation. The method comprises the following steps: respectively preparing a test solution and a series of magnesium element standard solutions, putting the test solution and the series of magnesium element standard solutions in an atomic absorption spectrophotometer to determine the absorbance, utilizing a standard curve process or a curvilinear equation to obtain the concentration of the test solution, and calculating to obtain an analysis result. An aqueous solution of nitric acid and a deionization agent solution are respectively added in the preparation of the test solution and the series of magnesium element standard solutions. The concentration of the lower detection limit of the method on the test solution is 0.005mug/ml, and the determination concentration is in a range of 0.007-1.5mug/ml. Compared with present common methods, the method disclosed in the invention has the advantages of less amount of a sample to be determined, rapidness, simplicity, less interference, high accuracy and the like.

Description

The content assaying method of magnesium elements in a kind of hydroxyethyl starch injection liquid preparation
Technical field
The present invention relates to a kind of content assaying method, particularly the content assaying method of magnesium elements in a kind of hydroxyethyl starch injection liquid preparation.
Background technology
Hydroxyethyl Starch (hydroxyethyl starch is called for short HES) is made after degraded, hydroxyethylation and further processing are processed by the high molecular amylopectin.Be blood volume expander.In order to improve Hemodynamics, microcirculation and oxygen supply function.Be used for treatment because of the shock of bleeding profusely, burning or other wound causing, apply to clinical as antishock basic therapy.
The composition of electrolyte that contains the elements such as the potassium that plays an important role with vital movement, sodium, calcium, magnesium during hydroxyethyl starch injection liquid prescription forms, it is a kind of hydroxyethyl starch injection liquid that contains the equilibrium electrolyte composition, this product has and does not change acid base equilibrium, reduces the hemostasis infringement, the support stomach pours into and keeps the characteristics such as renal function, be particularly suitable for prevention and treatment shock, have potential applicability in clinical practice widely.The hydroxyethyl starch injection liquid solution that contains the equilibrium electrolyte composition has electrolyte (sodium, potassium, calcium and magnesium) and the buffer composition to the similar concentration of blood plasma, as sodium lactate, sodium acetate and/or natrium malicum, and contain the chlorion that lacks than 0.9%NaCl solution, can not cause the disorder relevant with acid base equilibrium, this solution has the advantage of keeping better the cylinder electrolyte balance and reducing hemorrhagic tendency.The hydroxyethyl starch injection liquid that particularly contains the compositions such as sodium acetate and natrium malicum more is better than containing the hydroxyethyl starch injection liquid of sodium lactate composition, its reason is that exogenous lactate can not be by metabolism when shock, based on Lactated diagnosis, be specially adapted to prevention and treatment shock under meeting upset hypoxia.This solution has the advantage of keeping better the cylinder electrolyte balance and reducing hemorrhagic tendency.Owing to containing above more composition of electrolyte in hydroxyethyl starch injection liquid, when adopting conventional titrimetry, exist each other certain interference between each composition, therefore set up one easy, effectively, method detects the electrolyte analysis in prescription and seems particularly important accurately.
Summary of the invention
The object of the invention is to disclose the content assaying method of magnesium elements in a kind of hydroxyethyl starch injection liquid preparation.
The present invention seeks to be achieved through the following technical solutions.
In hydroxyethyl starch injection liquid preparation of the present invention, the content assaying method of electrolyte magnesium elements comprises the steps:
A. prepare test solution: get the hydroxyethyl starch injection liquid preparation in right amount in measuring bottle, add the deionized water dilution and make that to contain magnesium single element concentration be 0.007~1.5 μ g/ml, shake up, and get final product;
B. prepare magnesium single element series standard solution: the magnesium single element standard solution of getting concentration and be 1000 μ g/ml is appropriate, puts respectively in measuring bottle, is diluted to the magnesium single element standard solution that is complementary with test solution concentration with deionized water, shakes up, and get final product;
C. the test solution of steps A preparation and the magnesium single element series standard solution of step B preparation are measured absorbance simultaneously on atomic absorption spectrophotometer (AAS), utilize calibration curve method or curvilinear equation to obtain test fluid concentration, Calculation results.
Step B can specifically prepare as follows: the concentration magnesium single element standard solution that is 1000 μ g/ml is added deionized water, and to be diluted to magnesium single element concentration be 10 μ g/ml, as magnesium single element reference substance stock solution; Get respectively magnesium single element reference substance stock solution 1.0 parts by volume, 3.0 parts by volume, 5.0 parts by volume, 7.0 parts by volume, 9.0 parts by volume and put in measuring bottle, being diluted to magnesium single element concentration with deionized water is 1 * 10 -7G/ml, 3 * 10 -7G/ml, 5 * 10 -7G/ml, 7 * 10 -7G/ml, 9 * 10 -6G/ml shakes up, and get final product.
When the above-mentioned test solution of preparation and magnesium single element series standard solution, also can also add respectively nitric acid: the volume ratio of water is solution 0~10 parts by volume of 1: 1.Preferred 1~5 parts by volume.The mass concentration of described nitric acid is 35~72% (gram/grams).
When the above-mentioned test solution of preparation and magnesium single element series standard solution, also can by the conventional way of magnesium elements in test samples, add respectively ionization buffer solution 0~10 parts by volume of coupling, preferred 1~5 parts by volume.
The compound method of described ionization buffer solution is: take ionization buffer lanthanum chloride, strontium chloride, cesium chloride, lanthana, strontium oxide strontia or cesium oxide 1~15 weight portion in the measuring bottle of 100 parts by volume, make its dissolving and be diluted to scale with 0~10% (g/ml) salpeter solution (the acceptable salts acid solution substitutes), shake up, and get final product.Preferred compound method: take ionization buffer lanthanum chloride, strontium chloride, cesium chloride, lanthana, strontium oxide strontia or cesium oxide 2 weight portions in the measuring bottle of 100 parts by volume, make its dissolving and be diluted to scale with 5% salpeter solution, shake up, and get final product.
Described magnesium elements is the magnesium elements in magnesium chloride.the prescription of described hydroxyethyl starch injection liquid preparation consists of: Hydroxyethyl Starch (comprises Hydroxyethyl Starch/0.5, Hydroxyethyl Starch 130/0.4, Hydroxyethyl Starch 130/0.42), sodium chloride, potassium chloride (available potassium acetate, a kind of substituting in potassium malate or potassium citrate), magnesium chloride, sodium lactate (available sodium acetate, a kind of substituting in natrium malicum or sodium citrate), lime chloride (available calcium gluconate or calcium lactate substitute), glucose (or not containing glucose) etc.described hydroxyethyl starch injection liquid preparation can directly obtain from the selling market, include but not limited to: Hetastarch 200/0.5 sodium lactate ringer's injection, Hydroxyethyl Starch 130/0.4 sodium lactate ringer's injection, Hydroxyethyl Starch 130/0.4 sodium acetate ringer's injection, Hetastarch 200/0.5 sodium acetate ringer's injection, compound Hydroxyethyl Starch 130/0.4 sodium acetate ringer's injection, compound Hetastarch 200/0.5 sodium acetate ringer's injection, compound Hydroxyethyl Starch 130/0.4 electrolyte injection, compound Hetastarch 200/0.5 electrolyte injection.
The described instrument condition of step C can be Perkimelmer AAnalyst 800 type atomic absorption spectrophotometer (AAS)s, wavelength 285.2nm.
The analysis detecting data collection of enforcement the inventive method and the calculating of result data are with conventional Atomic absorption and spectrophotometric analysis data acquisition and computing method are close as a result, and computational analysis testing result concrete grammar is:
C X=ρ×N×10 -6
Wherein, C XBe tested parenteral solution concentration, g/ml
ρ: the mass concentration μ g/ml of the test solution that is calculated by typical curve or curvilinear equation
N: be extension rate
The unit corresponding relation of weight portion of the present invention and parts by volume is g/ml.
It is 0.005 μ g/ml that the inventive method detects least concentration to test fluid, and measuring concentration range is 0.007 μ g/ml~1.5 μ g/ml.Measure magnesium chloride relatively with existing argentometry commonly used or chromium titration, have that required test sample consumption is few (can be measured in atom spectrophotometric method Na ion concentration 0.007 μ g/ml~1.5 μ g/m scopes, the titrimetry least concentration is more than 100mg), fast, easy, disturb less, the accuracy advantages of higher, be applicable to the mensuration of micro-example.
Following experimental example and embodiment are used for further illustrating but being not limited to the present invention.
Experimental example: the determining of typical curve, repeatability and average recovery test
1. standard solution, ionization buffer solution, test solution preparation
Magnesium elements standard solution preparation: get magnesium single element standard solution (1000 μ g/ml) 1.0ml and add deionized water and be diluted to scale in the 100ml measuring bottle, as magnesium single element reference substance stock solution.Get respectively magnesium single element reference substance stock solution 1.0ml, 3.0ml, 5.0ml, 7.0ml, 9.0ml in the 100ml measuring bottle, respectively add ionization buffer solution 3ml, be diluted to scale with deionized water, shake up, and get final product.
Ionization buffer solution preparation: take cesium chloride 6.6g in the 100ml measuring bottle, make with deionized water and dissolve and be diluted to scale, shake up.
The test solution preparation: precision measures hydroxyethyl starch injection liquid 3.0ml, puts in the 100ml measuring bottle, adds ionization buffer solution 3ml, is diluted to scale with deionized water, shakes up, and get final product.
2. press step measurements, the drawing standard working curve of the inventive method
Adopt the inventive method at Perkimelmer AAnalyst 800 type atomic absorption spectrophotometer (AAS)s, wavelength 285.2nm place records the magnesium elements absorbance log, take tested elemental mass concentration as horizontal ordinate, absorbance log is ordinate drawing standard curve (as shown in Figure 1), and the relation of magnesium elements absorbance log and concentration sees Table 1.
The relation of table 1 magnesium elements Atomic absorption degree and concentration
3. sample determination
(1) in Hetastarch 200/0.5 sodium lactate ringer's injection, magnesium elements is measured
Measure carry out repeatedly (more than 5 times, below identical) with a collection of Hetastarch 200/0.5 sodium lactate ringer's injection by the described method of embodiment 1, calculate mean value, the relative standard deviation of measurement result.Measure magnesium elements accuracy in Hetastarch 200/0.5 sodium lactate ringer's injection for further investigating the method, get same batch sample, add certain magnesium standard solution, carry out the average recovery test, also repeatedly measure by above-mentioned sample determination step, data see Table 2.
Table 2
Element Measurement result mean value Relative standard deviation % Recovery %
Magnesium (g/ml) 0.011×10 -3 1.05 100.69
(2) in Hydroxyethyl Starch 130/0.4 sodium lactate ringer's injection, magnesium elements is measured
To repeatedly measuring with a collection of Hydroxyethyl Starch 130/0.4 sodium lactate ringer's injection, calculate mean value, the relative standard deviation of measurement result by the described method of embodiment 2.Measure magnesium elements accuracy in Hydroxyethyl Starch 130/0.4 sodium lactate ringer's injection for further investigating the method, get same batch sample, add certain magnesium standard solution, carry out the average recovery test, also repeatedly measure by above-mentioned sample determination step, data see Table 3.
Table 3
Element Measurement result mean value Relative standard deviation % Recovery %
Magnesium 0.010mg/ml 0.63 101.19
(3) in Hetastarch 200/0.5 sodium acetate ringer's injection, magnesium elements is measured
By the described method of embodiment 3 to repeatedly measuring with a collection of Hetastarch 200/0.5 sodium acetate ringer's injection, calculate mean value, the relative standard deviation of measurement result, measure magnesium elements accuracy in Hetastarch 200/0.5 sodium acetate ringer's injection for further investigating the method, get same batch sample, add certain magnesium standard solution, carry out the average recovery test, also repeatedly measure by above-mentioned sample determination step, data see Table 4.
Table 4
Element Measurement result mean value Relative standard deviation % Recovery %
Magnesium 0.024mg/ml 1.98 98.65
(4) in Hydroxyethyl Starch 130/0.4 sodium acetate ringer's injection, magnesium elements is measured
By the described method of embodiment 4 to repeatedly measuring with a collection of Hydroxyethyl Starch 130/0.4 sodium acetate ringer's injection, calculate mean value, the relative standard deviation of measurement result, measure magnesium elements accuracy in Hydroxyethyl Starch 130/0.4 sodium acetate ringer's injection for further investigating the method, get same batch sample, add certain magnesium standard solution, carry out the average recovery test, also repeatedly measure by above-mentioned sample determination step, data see Table 5.
Table 5
Element Measurement result mean value Relative standard deviation % Recovery %
Magnesium 0.026mg/ml 2.05 98.62
[0050](5) in compound Hetastarch 200/0.5 electrolyte injection, magnesium elements is measured
By the described method of embodiment 5, same reply side Hetastarch 200/0.5 electrolyte injection is repeatedly measured, calculate mean value, the relative standard deviation of measurement result, measure magnesium elements accuracy in compound Hetastarch 200/0.5 electrolyte injection for further investigating the method, get same batch sample, add certain magnesium standard solution, carry out the average recovery test, also repeatedly measure by above-mentioned sample determination step, data see Table 6.
Table 6
Element Measurement result mean value Relative standard deviation % Recovery %
Magnesium 0.020mg/ml 0.67 100.38
(6) in compound Hydroxyethyl Starch 130/0.4 electrolyte injection, magnesium elements is measured
By the described method of embodiment 6, same reply side Hydroxyethyl Starch 130/0.4 electrolyte injection is repeatedly measured, calculate mean value, the relative standard deviation of measurement result, measure magnesium elements accuracy in compound Hydroxyethyl Starch 130/0.4 electrolyte injection for further investigating the method, get same batch sample, add certain magnesium standard solution, carry out the average recovery test, also repeatedly measure by above-mentioned sample determination step, data see Table 7.
Table 7
Element Measurement result mean value Relative standard deviation % Recovery %
Magnesium 0.021mg/ml 1.09 99.36
Above (1)~(6) experimental result explanation, according to magnesium element content assay method of the present invention, to independent mensuration the on same sample 5 times, relative standard deviation is for all little by 3%, illustrate that the inventive method reappearance is better, sample is carried out recovery of standard addition test test findings show, the recovery is 98.62%~101.19%, illustrate that the inventive method has good accuracy and precision, method is accurately feasible.
Description of drawings:
The typical curve that Fig. 1 adopts the present invention to record with atomic absorption spectrophotometer (AAS).
Embodiment 1: magnesium element content assay method in Hetastarch 200/0.5 sodium lactate ringer's injection
A. prepare test solution: get Hetastarch 200/0.5 sodium lactate ringer's injection 3.0ml, put in the 100ml measuring bottle, add 2% cesium chloride solution 2ml, nitric acid: the volume ratio of water is the solution 1ml of 1: 1, is diluted to scale with deionized water, shakes up.
B. prepare magnesium single element series standard solution: get magnesium single element standard solution (1000 μ g/ml) 1.0ml and add deionized water and be diluted to scale, as magnesium single element reference substance stock solution in the 100ml measuring bottle.Get respectively magnesium single element reference substance stock solution 1.0ml, 2.0ml, 4.0ml, 6.0ml, 8.0m in the 100ml measuring bottle, respectively add 2% cesium chloride solution 2ml, nitric acid: the volume ratio of water is the solution 1ml of 1: 1, is diluted to scale with deionized water, shakes up, and get final product.
C. the instrument condition that adopts by table 1 is measured absorbance log simultaneously with magnesium single element series standard solution and test solution on atomic absorption spectrophotometer (AAS).According to absorbance in test solution, calculate test fluid concentration from aforesaid typical curve equation, calculate analysis result by aforesaid computing formula as follows:
C X = 0.334 × 100 3 × 10 - 6 = 0.011 × 10 - 3 g / ml
D.2% the preparation of cesium chloride solution: take ionization buffer cesium chloride 2g in the measuring bottle of 100ml, make its dissolving and be diluted to scale with 1% (g/ml) salpeter solution, shake up, and get final product.
Embodiment 2: magnesium element content assay method in Hydroxyethyl Starch 130/0.4 sodium lactate ringer's injection
A. prepare test solution: get Hydroxyethyl Starch 130/0.4 sodium lactate ringer's injection 5.0ml, put in the 100ml measuring bottle, add 2% cesium oxide solution 2ml, nitric acid: the volume ratio of water is the solution 5ml of 1: 1, is diluted to scale with deionized water, shakes up, and get final product.
B. prepare magnesium single element series standard solution: get magnesium single element standard solution (1000 μ g/ml) 1.0ml and add deionized water and be diluted to scale, as magnesium single element reference substance stock solution in the 100ml measuring bottle.Get respectively magnesium single element reference substance stock solution 1.0ml, 3.0ml, 5.0ml, 7.0ml, 9.0ml in the 100ml measuring bottle, respectively add 2% cesium oxide solution 2ml, hydrochloric acid: the volume ratio of water is the solution 5ml of 1: 1, is diluted to scale with deionized water, shakes up, and get final product.
C. the instrument condition that adopts by table 1 is measured absorbance log simultaneously with magnesium single element series standard solution and test solution on atomic absorption spectrophotometer (AAS).According to absorbance in test solution, calculate test fluid concentration from aforesaid typical curve equation, calculate analysis result by aforesaid computing formula as follows:
C X = 0 . 508 × 100 5 × 10 - 6 = 0 . 010 × 10 - 3 g / ml
D.2% the preparation of cesium oxide solution: take ionization buffer cesium oxide 2g in the measuring bottle of 100ml, make its dissolving and be diluted to scale with 3% (g/ml) hydrochloric acid solution, shake up, and get final product.
Embodiment 3: magnesium element content assay method in Hetastarch 200/0.5 sodium acetate ringer's injection
A. prepare test solution: get Hetastarch 200/0.5 sodium acetate ringer's injection 1.0ml, put in the 100ml measuring bottle, add 5% lanthanum chloride solution 7ml, be diluted to scale with deionized water, shake up.
B. prepare magnesium series standard solution: get magnesium single element standard solution (1000 μ g/ml) 1.0ml and add deionized water and be diluted to scale, as magnesium single element reference substance stock solution in the 100ml measuring bottle.Get respectively magnesium single element reference substance stock solution 1.0ml, 2.0ml, 3.0ml, 4.0ml, 5.0ml in the 100ml measuring bottle, respectively add 5% lanthanum chloride solution 7ml, be diluted to scale with deionized water, shake up, and get final product.
C. the instrument condition that adopts by table 1 is measured absorbance log simultaneously with magnesium single element series standard solution and test solution on atomic absorption spectrophotometer (AAS).According to absorbance in test solution, calculate test fluid concentration from aforesaid typical curve equation, calculate analysis result by aforesaid computing formula as follows:
C X = 0 . 242 × 100 1 × 10 - 6 = 0.024 × 10 - 3 g / ml
D.5% the preparation of lanthanum chloride solution: take ionization buffer lanthanum chloride 5g in the measuring bottle of 100ml, make its dissolving and be diluted to scale with 5% (g/ml) salpeter solution, shake up, and get final product.
Embodiment 4: magnesium element content assay method in Hydroxyethyl Starch 130/0.4 sodium acetate ringer's injection
A. prepare test solution: get Hydroxyethyl Starch 130/0.4 sodium acetate ringer's injection 20.0ml, put in the 100ml measuring bottle, add deionized water and be diluted to scale, precision measures 8ml, put in the 100ml measuring bottle, add 10% lanthana solution 10ml, nitric acid: the volume ratio of water is the solution 3ml of 1: 1, be diluted to scale with deionized water, shake up.
B. prepare magnesium series standard solution: get magnesium single element standard solution (1000 μ g/ml) 1.0ml and add deionized water and be diluted to scale, as magnesium single element reference substance stock solution in the 100ml measuring bottle.Get respectively magnesium single element reference substance stock solution 1.0ml, 2.0ml, 3.0ml, 4.0ml, 5.0ml in the 100ml measuring bottle, respectively add 10% lanthana solution 10ml, nitric acid: the volume ratio of water is the solution 3ml of 1: 1, is diluted to scale with deionized water, shake up, and get final product.
C.. the instrument condition that adopts by table 1 is measured absorbance log simultaneously with magnesium single element series standard solution and test solution on atomic absorption spectrophotometer (AAS).According to absorbance in test solution, calculate test fluid concentration from aforesaid typical curve equation, calculate analysis result by aforesaid computing formula:
C X = 0 . 416 × 100 20 × 100 8 × 10 - 6 = 0.026 × 10 - 3 g / ml
D.10% the preparation of lanthana solution: take ionization buffer lanthana 10g in the measuring bottle of 100ml, make its dissolving and be diluted to scale with 5% (g/ml) hydrochloric acid solution, shake up, and get final product.
Embodiment 5: magnesium element content assay method in compound Hetastarch 200/0.5 electrolyte injection
A. prepare test solution: get compound Hetastarch 200/0.5 electrolyte injection 4.0ml, put in the 100ml measuring bottle, add 15% strontium chloride solution 1ml, be diluted to scale with deionized water, shake up.
B. prepare magnesium single element series standard solution: get magnesium single element standard solution (1000 μ g/ml) 1.0ml and add deionized water and be diluted to scale, as magnesium single element reference substance stock solution in the 100ml measuring bottle.Get respectively magnesium single element reference substance stock solution 1.0ml, 3.0ml, 5.0ml, 7.0ml, 9.0ml in the 100ml measuring bottle, respectively add 15% strontium chloride solution 1ml, be diluted to scale with deionized water, shake up, and get final product.
C. the instrument condition that adopts by table 1 is measured absorbance log simultaneously with magnesium series standard solution and test solution on atomic absorption spectrophotometer (AAS).According to absorbance in test solution, calculate test fluid concentration from aforesaid typical curve equation, calculate analysis result by aforesaid computing formula:
C X = 0 . 806 × 100 4 × 10 - 6 = 0.020 × 10 - 3 g / ml
D.15% the preparation of strontium chloride solution: take ionization buffer strontium chloride 15g in the measuring bottle of 100ml, make its dissolving and be diluted to scale with salpeter solution, shake up, and get final product.
Embodiment 6: magnesium element content assay method in compound Hydroxyethyl Starch 130/0.4 electrolyte injection
A. prepare test solution: get compound Hydroxyethyl Starch 130/0.4 electrolyte injection 25.0ml, put in the 100ml measuring bottle, add deionized water and be diluted to scale, precision measures 2ml, put in the 100ml measuring bottle, add 6.6% strontium oxide strontia solution 5ml, nitric acid: the volume ratio of water is the solution 10ml of 1: 1, be diluted to scale with deionized water, shake up.
B. prepare magnesium series standard solution: get magnesium single element standard solution (1000 μ g/ml) 1.0ml and add deionized water and be diluted to scale, as magnesium single element reference substance stock solution in the 100ml measuring bottle.Get respectively magnesium single element reference substance stock solution 1.0ml, 3.0ml, 5.0ml, 7.0ml, 9.0ml in the 100ml measuring bottle, respectively add 6.6% strontium oxide strontia solution 5ml, nitric acid: the volume ratio of water is the solution 10ml of 1: 1, is diluted to scale with deionized water, shake up, and get final product.
C. the instrument condition that adopts by table 1 is measured absorbance log simultaneously with magnesium single element series standard solution and test solution on atomic absorption spectrophotometer (AAS).According to absorbance in test solution, calculate test fluid concentration from aforesaid typical curve equation, calculate analysis result by aforesaid computing formula:
C X = 0 . 105 × 100 25 × 100 2 × 10 - 6 = 0 . 021 × 10 - 3 g / ml
D.6.6% the preparation of strontium oxide strontia solution: take ionization buffer strontium oxide strontia 6.6g in the measuring bottle of 100ml, make its dissolving and be diluted to scale with 10% hydrochloric acid solution, shake up, and get final product.
Embodiment 7: compound Hetastarch 200/0.5 sodium acetate ringer's injection
A. prepare test solution: get compound Hetastarch 200/0.5 sodium acetate ringer's injection 30.0ml, put in the 100ml measuring bottle, be diluted to scale with deionized water, precision measures 20.0ml in the 100ml measuring bottle, adds deionized water and is diluted to scale, shakes up, and get final product.
B. prepare magnesium series standard solution: get magnesium single element standard solution (1000 μ g/ml) 1.0ml and add deionized water and be diluted to scale, as magnesium single element reference substance stock solution in the 100ml measuring bottle.Get respectively magnesium single element reference substance stock solution 1.0ml, 3.0ml, 5.0ml, 10.0ml, 15.0ml in the 100ml measuring bottle, be diluted to scale with deionized water, shake up, and get final product.
C. adopt the TAS-986 atomic absorption spectrophotometer (AAS), wavelength 285.2nm place measures absorbance log simultaneously with magnesium single element series standard solution and test solution on atomic absorption spectrophotometer (AAS).According to absorbance in test solution, calculate test fluid concentration from aforesaid typical curve equation, calculate analysis result by aforesaid computing formula as follows:
C X = 1.441 × 100 30 × 100 20 × 10 - 6 = 0.024 × 10 - 3 g / ml
Embodiment 8: in compound Hydroxyethyl Starch 130/0.4 sodium acetate ringer's injection, magnesium elements is measured
A. prepare test solution: get compound Hydroxyethyl Starch 130/0.4 sodium acetate ringer's injection 5.0ml, put in the 100ml measuring bottle nitric acid: the volume ratio of water is the solution 3ml of 1: 1, is diluted to scale with deionized water, shakes up.
B. prepare magnesium series standard solution: get magnesium single element standard solution (1000 μ g/ml) 1.0ml and add deionized water and be diluted to scale, as magnesium single element reference substance stock solution in the 100ml measuring bottle.Get respectively magnesium single element reference substance stock solution 1.0ml, 3.0ml, 5.0ml, 10.0ml, 15.0ml in the 100ml measuring bottle, respectively add 10% lanthana solution 10.0ml, nitric acid: the volume ratio of water is the solution 3ml of 1: 1, is diluted to scale with deionized water, shake up, and get final product.
C. adopt the TAS-986 atomic absorption spectrophotometer (AAS), wavelength 285.2nm place measures absorbance log simultaneously with magnesium single element series standard solution and test solution on atomic absorption spectrophotometer (AAS).According to absorbance in test solution, calculate test fluid concentration from aforesaid typical curve equation, calculate analysis result by aforesaid computing formula:
C X = 1.312 × 100 5 × 10 - 6 = 0.026 × 10 - 3 g / ml

Claims (11)

1. the content assaying method of electrolyte magnesium elements in a hydroxyethyl starch injection liquid preparation, is characterized in that the method comprises the steps:
A. prepare test solution: get the hydroxyethyl starch injection liquid preparation in right amount in measuring bottle, add the deionized water dilution and make that to contain magnesium single element concentration be 0.007~1.5 μ g/ml, shake up, and get final product;
B. prepare magnesium single element series standard solution: the magnesium single element standard solution of getting concentration and be 1000 μ g/ml is appropriate, puts respectively in measuring bottle, is diluted to the magnesium single element standard solution that is complementary with test solution concentration with deionized water, shakes up, and get final product;
C. the test solution of steps A preparation and the magnesium single element series standard solution of step B preparation are measured absorbance simultaneously on atomic absorption spectrophotometer (AAS), utilize calibration curve method or curvilinear equation to obtain test fluid concentration, Calculation results.
2. the content assaying method of electrolyte magnesium elements in hydroxyethyl starch injection liquid preparation as claimed in claim 1, it is characterized in that step B prepares as follows: the concentration magnesium single element standard solution that is 1000 μ g/ml is added deionized water, and to be diluted to magnesium single element concentration be 10 μ g/ml, as magnesium single element reference substance stock solution; Get respectively magnesium single element reference substance stock solution 1.0 parts by volume, 3.0 parts by volume, 5.0 parts by volume, 7.0 parts by volume, 9.0 parts by volume and put in measuring bottle, being diluted to magnesium single element concentration with deionized water is 1 * 10 -7G/ml, 3 * 10 -7G/ml, 5 * 10 -7G/ml, 7 * 10 -7G/ml, 9 * 10 -6G/ml shakes up, and get final product.
3. the content assaying method of electrolyte magnesium elements in hydroxyethyl starch injection liquid preparation as claimed in claim 1, it is characterized in that also can add respectively nitric acid: the volume ratio of water is solution 0~10 parts by volume of 1: 1 when preparation test solution or magnesium single element series standard solution.
4. the content assaying method of electrolyte magnesium elements in hydroxyethyl starch injection liquid preparation as claimed in claim 3, it is characterized in that described nitric acid: the volume ratio of water is that the solution of 1: 1 is 1~5 parts by volume.
5. the content assaying method of electrolyte magnesium elements in hydroxyethyl starch injection liquid preparation as claimed in claim 1, is characterized in that also adding respectively ionization buffer solution 0~10 parts by volume when preparation test solution or magnesium single element series standard solution.
6. the content assaying method of electrolyte magnesium elements in hydroxyethyl starch injection liquid preparation as claimed in claim 5, is characterized in that described ionization buffer solution is 1~5 parts by volume.
7. the content assaying method of electrolyte magnesium elements in hydroxyethyl starch injection liquid preparation as claimed in claim 5, the compound method that it is characterized in that described ionization buffer solution is: take ionization buffer lanthanum chloride, strontium chloride, cesium chloride, lanthana, strontium oxide strontia or cesium oxide 1~15 weight portion in the measuring bottle of 100 parts by volume, make its dissolving and be diluted to scale with 0~10% nitric acid or hydrochloric acid solution, shake up, and get final product.
8. the content assaying method of electrolyte magnesium elements in hydroxyethyl starch injection liquid preparation as claimed in claim 7, the compound method that it is characterized in that described ionization buffer solution is: take ionization buffer lanthanum chloride, strontium chloride, cesium chloride, lanthana, strontium oxide strontia or cesium oxide 2 weight portions in the measuring bottle of 100 parts by volume, make its dissolving and be diluted to scale with 5% salpeter solution, shake up, and get final product.
9. as the content assaying method of electrolyte magnesium elements in any one hydroxyethyl starch injection liquid preparation as described in claim 1~8, it is characterized in that the described instrument condition of step C is: Perkimelmer AAnalyst 800 atomic absorption spectrophotometer (AAS)s, wavelength 285.2nm.
10. as the content assaying method of electrolyte magnesium elements in any one hydroxyethyl starch injection liquid preparation as described in claim 1~8, it is characterized in that described magnesium elements is the magnesium elements in magnesium chloride.
11. the content assaying method as electrolyte magnesium elements in any one hydroxyethyl starch injection liquid preparation as described in claim 1~8, it is characterized in that described hydroxyethyl starch injection liquid preparation comprises: Hetastarch 200/0.5 sodium lactate ringer's injection, Hydroxyethyl Starch 130/0.4 sodium lactate ringer's injection, Hydroxyethyl Starch 130/0.4 sodium acetate ringer's injection, Hetastarch 200/0.5 sodium acetate ringer's injection, compound Hydroxyethyl Starch 130/0.4 sodium acetate ringer's injection, compound Hetastarch 200/0.5 sodium acetate ringer's injection, compound Hydroxyethyl Starch 130/0.4 electrolyte injection or compound Hetastarch 200/0.5 electrolyte injection.
CN2011104293737A 2011-12-20 2011-12-20 Method for determining content of magnesium element in hydroxyethyl starch injection preparation Pending CN103175802A (en)

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