CN103575669A - Method for measuring content of potassium chloride and sodium chloride in potassium chloride and sodium chloride injection solution - Google Patents
Method for measuring content of potassium chloride and sodium chloride in potassium chloride and sodium chloride injection solution Download PDFInfo
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Abstract
The invention relates to a method for measuring the content of potassium chloride and sodium chloride in a potassium chloride and sodium chloride injection solution, and a method for determining whether the content of potassium chloride and sodium chloride in the potassium chloride and sodium chloride injection solution meets quality standards. The measuring method is carried out through an atomic absorption spectrometry method by an atomic absorption spectrophotometer.
Description
Technical field
The present invention relates to a kind of potassium chloride of potassium chloride in sodium chloride inj and the assay method of sodium chloride content, and whether the potassium chloride of definite potassium chloride in sodium chloride inj and sodium chloride content meet the method for quality standard.
Background technology
Potassium chloride (KCl) is one of most basic clinical application, is national basic medical medication catalogue product, national social security catalogue product; Be mainly used in treating all kinds of hypopotassaemias, in each large, medium and small hospital, for a long time, extensively use.Described in the 17 edition the 157th page, Merck diagnosis and treatment handbook: in order to supplement KCl, Glucose Liquid is not ideal chose, because increase subsequently patient's plasma insulin level, can cause the property a crossed hypopotassaemia to increase the weight of, symptom aggravation, particularly digitalis patient.Finally, when hypopotassaemia is with low magnesium, conventionally need to correct the prevention of magnesium shortage and contain potassium loss and impel potassium full." domesticly also have bibliographical information " because the input of glucose has, to make K when the synthetic glycogen
+enter cell, fall hypokalemic phenomenon, 10% glucose also has osmotic diuresis effect, therefore do the dilution of potassium chloride injection with 10% glucose, has improper part.
Current domestic listing KCl preparation mainly contains: (1) oral tablet, be mainly used in the outpatient of light disease hypopotassaemia and without disease of digestive tract person: (2) KCl injection, existing commercially available potassium chloride parenteral solution specification is 10ml: 1.5g and 1.0g, clinical in serious hypopotassaemia or can not oral person.According to the clinical administration method of describing in " 10ml: 1.5g " specification liquid drugs injection product description, be: be generally 15% potassium chloride parenteral solution 7-10ml to be added in 5% glucose injection 500ml to instil (avoid direct drip-feed and inject).Therefore, in actual use procedure, likely produce secondary pollution.
In Chinese Pharmacopoeia, in compound sodium chloride injection, the assay of potassium chloride adopts Sodium Tetraphenylborate Method, this method operating performance is numerous and diverse and time-consuming, sodium chloride content is measured and is adopted argentometry, in practical operation, often due to the not obvious error that causes of titration end-point hop phenomenon.
In order to address the above problem, need a kind of new potassium chloride injection, and set up a kind of content assaying method accurately, the mensuration that provides science for the quality control of this product according to and obtain measurement result accurately.
Summary of the invention
In order to solve the problems referred to above in the use procedure of potassium chloride parenteral solution, applicant has developed a kind of novel form of KCl parenteral solution, i.e. potassium chloride in sodium chloride inj.Meanwhile, for controlling the quality of potassium chloride in sodium chloride inj, adopt atomic absorption spectrophotometer (AAS) to measure by atomic absorption spectrophotometry.And the method can be carried out METHOD FOR CONTINUOUS DETERMINATION to the potassium chloride in potassium chloride in sodium chloride inj and sodium chloride content.And, according to the measurement result of the method, can judge whether potassium chloride and the sodium chloride content in potassium chloride in sodium chloride inj meets quality standard.
The invention provides following three kinds of specifications, can use flexibly according to clinical needs:
(1) 100mL: the potassium chloride in sodium chloride inj of potassium chloride 0.11g and sodium chloride 0.9g;
(2) 100mL: the potassium chloride in sodium chloride inj of potassium chloride 0.22g and sodium chloride 0.9g;
(3) 100mL: the potassium chloride in sodium chloride inj of potassium chloride 0.11g and sodium chloride 0.9g.
With traditional KCl injection comparison, without dilution before use, easy to use, reduced the chance of secondary pollution.And owing to take sodium chloride solution as carrier, sugar-free can be used in the hyperglycemia patients such as diabetes.
The present invention adopts atomic absorption spectrophotometry to measure the content of potassium chloride and sodium chloride.The ultimate principle of atomic absorption spectroscopy is to measure the absorption of ground state atom to resoance radiation.For the content of Accurate Determining potassium chloride and sodium chloride need to carry out fine adjustment and selection to the parameter of atomic absorption spectrophotometer (AAS).The purity of institute's water has a significant impact analyzing measurement result, and unpurified water can pollute testing sample and affect measurement result, in addition, for the impurity effect measurement result in anti-sealing, need to use ultrapure water.Applicant determines through great many of experiments, uses following parameter can obtain optimum determining result: for the mensuration of KCE content, and lamp current: 12.0mA; Slit: 1.3nm; Wavelength: 766.5nm; And burner height: 7.5mm.For the mensuration of sodium chloride content, lamp current: 12.0mA; Slit: 0.4nm; Wavelength: 589.0nm; And burner height: 7.5mm.Meanwhile, the ultrapure water that use resistivity is 18M Ω CM is as solvent.
Method of the present invention is measured the KCE content of potassium chloride in sodium chloride inj, if to measure the KCE content that obtains be labelled amount 95.0%～105.0%, this potassium chloride in sodium chloride inj meets quality standard.
Method of the present invention is measured the sodium chloride content of potassium chloride in sodium chloride inj, if to measure the sodium chloride content that obtains be labelled amount 95.0%～105.0%, this potassium chloride in sodium chloride inj meets quality standard.
With said method, measure, can obtain lower detection limit, the present invention is described compared with prior art, there is better technical advantage.
In addition, in assay method in the past, conventionally by product solution in contrast after titer dilution.But, applicant's discovery, when the potassium chloride in measuring potassium chloride in sodium chloride inj and the content of sodium chloride, sodion and potassium ion can influence each other, and have reduced the accuracy of measurement result.For fear of above-mentioned impact, when measuring KCE content, the present invention adds sodium chloride solution in reference substance solution, to eliminate the interference of sodion to K+ determination; When measuring sodium chloride content, the present invention adds Klorvess Liquid in reference substance solution, the interference of sodion being measured to eliminate potassium ion.The result of doing is like this accuracy that has farthest guaranteed measurement result.In the selection of reference substance solution, the sample of keeping off for the amount of potassium chloride and sodium chloride, if all use same reference substance solution, can produce very large error, even obtains wrong result.That is to say, for different samples, the sample that especially amount of potassium chloride and sodium chloride is kept off, need to prepare different reference substance solution according to the situation of specific product, just can obtain result accurately.In addition, the application mainly measures the potassium chloride in sodium chloride inj of following specification
(1) 100mL: the potassium chloride in sodium chloride inj of potassium chloride 0.11g and sodium chloride 0.9g;
(2) 100mL: the potassium chloride in sodium chloride inj of potassium chloride 0.22g and sodium chloride 0.9g; Or
(3) 100mL: the potassium chloride in sodium chloride inj of potassium chloride 0.11g and sodium chloride 0.9g.
In order to measure the concentration of two kinds of components in solution simultaneously, those skilled in the art may expect mixing to obtain the potassium chloride concentration a series of reference substance solution different with sodium chloride concentration with potassium chloride standard solution and sodium chloride standard solution, then measure the concentration of potassium chloride and the concentration of sodium chloride in potassium chloride in sodium chloride inj according to this series reference substance solution.But above method also reckons without the phase mutual interference between potassium ion and sodion.Applicant finds, because sodion under variable concentrations is different and different with concentration from the phase mutual interference of potassium ion.In certain concentration range, need to eliminate this interference with potassium ion and the sodion of specified quantitative.Otherwise cannot Accurate Measurement KCE content and sodium chloride content.Particularly, for above-mentioned specification of the present invention, when measuring KCE content, using sodium chloride solution as blank test solution, its preparation method is as follows: by 0.7g～1.1g sodium chloride, and preferred 0.8～1.0g sodium chloride, more preferably 0.9g sodium chloride is dissolved in water and is diluted to 100mL, shake up, precision measures gained solution 5.0mL, is placed in 50mL measuring bottle, is diluted with water to scale, shake up, obtain blank test solution.Simultaneously, when measuring sodium chloride content, using Klorvess Liquid as blank test solution, its preparation method is as follows: by 0.1g～0.5g potassium chloride, preferred 0.2～0.4g potassium chloride, more preferably 0.3g potassium chloride is dissolved in water and is diluted to 100mL, shakes up, and precision measures gained solution 5.0mL, be placed in 100mL measuring bottle, be diluted with water to scale, shake up, obtain blank test solution.Thus, can realize technique effect of the present invention.
In the present invention, KCE content is measured and to be compared with Sodium Tetraphenylborate Method in pharmacopeia, have simple to operate, quick, sampling amount is few, result is advantage accurately, has met the needs of pharmaceutical factory and hospital's express-analysis, the while can be carried out quality control to pharmaceutical production.In the present invention, sodium chloride content is measured and to be compared with argentometry, the error that does not have the control of titration end-point to bring, measurement result is more accurate, and method is simpler, fast.
The present invention adopts atomic absorption spectroscopy determination potassium chloride and sodium chloride content, has effectively controlled the real content of two kinds of salt, easy and simple to handle, and the recovery is satisfied.
Accompanying drawing explanation
Fig. 1 is potassium ion typical curve;
Fig. 2 is sodion typical curve.
Embodiment
In assay method of the present invention, first prepare the standard solution of potassium chloride or sodium chloride.This standard solution can be buied, for example, from ferrous materials test center of Iron and Steel Research Geueral Inst country, buy, and also can prepare voluntarily.Subsequently, by standard solution and blank test solution, prepare reference substance solution.Then by testing sample, prepare need testing solution.Finally adopt atomic absorption spectrophotometry to measure.
When measuring the KCE content of potassium chloride in sodium chloride inj, applicant, by great many of experiments, has determined the setup parameter of atomic absorption spectrophotometer (AAS), and these parameters are the principal elements that affect sensitivity and stability.Wherein lamp current is 7～12mA.If lamp current is too high, easily produce self-priming effect, Doppler effect strengthens, and line broadening is measured sensitivity, the lamp lost of life.But lamp current is too low, luminous intensity weakens, and spectral line signal to noise ratio (S/N ratio) reduces.Preferably lamp current is 12.0mA.Slit is 1.3nm or 0.4nm, is preferably 1.3nm.Slit is set wide, and signal to noise ratio (S/N ratio) is good, but differentiates rate variance; Slit is set narrow, good resolution, but signal to noise ratio (S/N ratio) decline answers both to take into account.Wavelength is 766.5nm.Burner height is 5～10mm, is preferably 7.5mm.Burner height difference temperature is different.By limiting above parameter, can measure more exactly KCE content.
When measuring the sodium chloride content of potassium chloride in sodium chloride inj, applicant, equally by great many of experiments, has determined the setup parameter of atomic absorption spectrophotometer (AAS).Wherein lamp current is 8～12mA.Preferably lamp current is 12.0mA.Slit is 0.4nm or 1.3nm, is preferably 0.4nm.Wavelength is 589.0nm.Burner height is 5～10mm, is preferably 7.5mm.By limiting above parameter, can measure more exactly sodium chloride content.
In addition, because sodion and potassium ion can influence each other, reduced the accuracy of measurement result, for fear of above-mentioned impact, when measuring KCE content, the present invention adds sodium chloride solution in reference substance solution, to eliminate the interference of sodion to K+ determination; When measuring sodium chloride content, the present invention adds Klorvess Liquid in reference substance solution, the interference of sodion being measured to eliminate potassium ion.Applicant has found that by great many of experiments (for potassium chloride concentration, measure, be the concentration of sodium chloride blank test solution to the concentration of the most suitable blank test solution in reference substance solution; For sodium chloride concentration, measuring, is the concentration of potassium chloride blank test solution), rather than the identical reference substance solution of use without exception, thus guaranteed the accuracy of measurement result, improved mensuration precision simultaneously.
Illustrate by the following examples assay method of the present invention fast, accurately, easily operation, and precision is high, data accurately and reliably, are applicable to potassium chloride and sodium chloride content in potassium chloride in sodium chloride inj and measure.
Embodiment
In the present invention, Z-5000 atomic absorption spectrophotometer (AAS) (Hitachi, Ltd) can be used, and AE240 electronic balance (Mei Tele company) (sensibility reciprocal: 0.01mg) weigh can be used.
The mensuration of embodiment 1 KCE content
1) preparation of blank test solution:
0.9g sodium chloride be dissolved in water and be diluted to 100mL, shaking up, precision measures gained solution 5.0mL, is placed in 50mL measuring bottle, is diluted with water to scale, shakes up, and obtains blank test solution;
2) preparation of reference substance solution:
It is potassium standard solution ([national standard solution GBSG 62020-90 (2601)] national ferrous materials test center that 1000 μ g/mL, medium are 10%HCl that precision measures concentration, Iron and Steel Research Geueral Inst) 5.0mL, be placed in 50mL measuring bottle, be diluted with water to scale, shake up, obtain the solution that concentration is 100 μ g/mL, precision measures solution 1.0mL, 2.0mL, 3.0mL, 4.0mL and the 5.0mL of 100 μ g/mL, be placed in respectively 100mL measuring bottle, precision adds blank test solution 5.0mL again, be diluted with water to scale, shake up, obtain reference substance solution;
3) preparation of need testing solution:
Precision measures testing sample, and thin up is made the potassium ion solution that concentration is 3 μ g/mL, obtains need testing solution;
4) measure:
Adopt the absorbance of atomic absorption spectroscopy determination reference substance solution and need testing solution, condition determination: detect wavelength 766.5nm, lamp current: 12.0mA; Slit: 1.3nm; And burner height: 7.5mm.Detect the absorbance of reference substance solution, drawing standard curve (seeing Fig. 1); Detect the absorbance of need testing solution, from typical curve, check in the concentration of need testing solution, calculate content, the concentration * extension rate/labelled amount of content=check in.
In above step, the water using derives from Milli-Q ultrapure water system (resistivity is 18M Ω CM).
5. detection limit and quantitative limit
Get blank test solution, adopt atomic absorption spectrophotometry, at lamp current: 12.0mA; Slit: 1.3nm; Wavelength: 766.5nm; Under the condition of and burner height: 7.5mm, measure absorbance, METHOD FOR CONTINUOUS DETERMINATION 20 times, the standard deviation that calculates 20 blank values is 0.0004 (Abs).
Detection limit=3s/b=3 * 4 * 10
-4/ 8.872 * 10
-2=1.35 * 10
-2(μ g/mL)
Quantitative limit=3.3 * detection limit=3.3 * 1.35 * 10
-2=4.46 * 10
-2(μ g/mL)
6. linearity
Precision measures reference substance solution, by above-mentioned condition, detects, and result is as shown in table 1.
Table 1 potassium ion is linear
| Concentration (μ g/mL) | 1.0 | 2.0 | 3.0 | 4.0 | 5.0 |
| Absorbance (Abs) | 0.0980 | 0.1915 | 0.2830 | 0.3753 | 0.4497 |
Take absorbance (abs) as ordinate (Y), and concentration is horizontal ordinate (X), calculates regression equation to be: Y=8.872 * 10
-2x+1.334 * 10
-2, r=0.9992.Illustrate that potassium ion is in the scope of 1 μ g/mL～5 μ g/mL, the linear relationship of concentration and absorbance is good.
Take absorbance (abs) as ordinate (Y), and the concentration of potassium ion (μ g/mL) is horizontal ordinate (X), and drawing standard curve, is shown in Fig. 1.
7. precision
Get lot number and be 090401 sample (100mL: potassium chloride 0.11g and sodium chloride 0.9g) as test specimen, according to above-mentioned condition, test, METHOD FOR CONTINUOUS DETERMINATION 5 times, measurement result is in Table 2.
The test of table 2 accuracy
| Measure number of times | 1 | 2 | 3 | 4 | 5 |
| Absorbance (Abs) | 0.2839 | 0.2834 | 0.2826 | 0.2844 | 0.2746 |
Same need testing solution replication 5 times, result mean value is 0.2818, relative standard deviation (RSD%) is 1.44%, meets mensuration requirement.
8. method reappearance
Get lot number and be 5 parts, 090401 sample (100mL: potassium chloride 0.11g and sodium chloride 0.9g), according to above-mentioned condition, test, measurement result is in Table 3.
The test of table 3 reappearance
| Numbering | 1 | 2 | 3 | 4 | 5 | 6 |
| Absorbance (Abs) | 0.2792 | 0.2771 | 0.2778 | 0.2748 | 0.2731 | 0.2784 |
Same lot number sample replication 5 times, result mean value is 0.2767, relative standard deviation (RSD%) is 0.84%, illustrates that this method reappearance is good.
9. test liquid stability
Get lot number and be 090401 sample (100mL: potassium chloride 0.11g and sodium chloride 0.9g) as need testing solution, measure respectively 0,1,2,4,8 hour above-mentioned condition of photograph, measurement result is in Table 4.
Table 4 stability test
| Time (h) | 0 | 1 | 2 | 4 | 8 |
| Absorbance (Abs) | 0.2791 | 0.2764 | 0.2795 | 0.2809 | 0.2755 |
Result mean value is 0.2783, and relative standard deviation (RSD%) is 0.81%, and the above results shows that need testing solution measured more stablely in 8 hours, can meet the needs of measuring.
10. the recovery:
Precision measures potassium standard solution (100 μ g/mL) 2.4mL, 3.0mL, 3.6mL, splits in 100mL measuring bottle, then precision measures blank test solution, and [sodium chloride 0.9g is dissolved in water and is diluted to 100mL, shakes up.Precision measures above-mentioned solution 5.0mL and puts in 50mL measuring bottle, is diluted with water to scale, shakes up] 2.0mL, be diluted with water to scale, shake up.By above-mentioned condition, detect, result is as shown in table 5.
Table 5: recovery test
| Numbering | Addition (μ g/ml) | Absorbance (Abs) | The amount of recording (μ g/ml) | The recovery (%) |
| 1 | 2.40 | 0.2260 | 2.3964 | 99.85 |
| 2 | 2.40 | 0.2255 | 2.3908 | 99.62 |
| 3 | 2.40 | 0.2298 | 2.4393 | 101.64 |
| 4 | 3.00 | 0.2821 | 3.0287 | 100.96 |
| 5 | 3.00 | 0.2847 | 3.0581 | 101.94 |
| 6 | 3.00 | 0.2862 | 3.0750 | 102.50 |
| 7 | 3.60 | 0.3408 | 3.6904 | 102.51 |
| 8 | 3.60 | 0.3399 | 3.6803 | 102.23 |
| 9 | 3.60 | 0.3420 | 3.7039 | 102.89 |
As seen from the above table, the recovery of nine test samples is between 99.62%～102.51%, and average recovery rate is that 101.57%, RSD is 1.16%, shows that this determination method can determine the content of potassium ion in sample exactly, and method is feasible.
The assay result of 11. 3 batch samples
In three batch samples that are 090401～090403 at lot number, get each test agent in three parts of each lot number, pressing potassium chloride in sodium chloride inj content assaying method measures, obtain on typical curve, finding corresponding concentration after absorbance, according to the concentration * extension rate/labelled amount of: content=check in, calculate content, it the results are shown in Table 6.
KCE content measurement result in table 6 sample
Therefore, according to this measurement result, three batch sample potassium chloride (KCl) content of described three kinds of specifications are labelled amount 97.9～104.4%, up to specification 95.0～105.0%.
The mensuration of embodiment 2 sodium chloride contents
1) preparation of blank test solution:
Potassium chloride 0.3g be dissolved in water and be diluted to 100mL, shaking up, precision measures gained solution 5.0mL, is placed in 100mL measuring bottle, is diluted with water to scale, shakes up, and obtains blank test solution;
2) preparation of reference substance solution:
It is sodium standard solution ([national standard solution GBSG 62020-90 (2601)] national ferrous materials test center that 1000 μ g/mL, medium are 10%HCl that precision measures concentration, Iron and Steel Research Geueral Inst) 5.0mL, be placed in 100mL measuring bottle, be diluted with water to scale, shake up, obtain the solution that concentration is 50 μ g/mL, precision measures solution 1.0mL, 2.0mL, 3.0mL, 4.0mL and the 5.0mL of 50 μ g/mL, be placed in respectively 100mL measuring bottle, precision adds blank test solution 1.0mL again, be diluted with water to scale, shake up, obtain reference substance solution;
3) preparation of need testing solution:
Precision measures testing sample, and thin up is made the sodion solution that concentration is 1.8 μ g/mL, obtains need testing solution;
4) measure:
The absorbance that adopts atomic absorption spectroscopy determination reference substance solution and need testing solution, condition determination is: detect wavelength 589.0nm; Lamp current: 12.0mA; Slit: 0.4nm; Wavelength: 589.0nm; And burner height: 7.5mm.Detect the absorbance of reference substance solution, drawing standard curve (seeing Fig. 2); Detect the absorbance of need testing solution, from typical curve, check in the concentration of need testing solution, calculate content, the concentration * extension rate/labelled amount of content=check in.
In above step, the water using derives from Milli-Q ultrapure water system (resistivity is 18M Ω CM).
5. detection limit and quantitative limit
Get blank test solution, adopt atomic absorption spectrophotometry, at lamp current: 12.0mA; Slit: 0.4nm; Wavelength: 589.0nm; Under the condition of and burner height: 7.5mm, measure absorbance, METHOD FOR CONTINUOUS DETERMINATION 20 times, the standard deviation that calculates 20 blank values is 2.5 * 10-3 (Abs).
Detection limit=3s/b=3 * 2.5 * 10
-3/ 2.149 * 10
-1=3.49 * 10
-2(μ g/mL)
Quantitative limit=3.3 * detection limit=3.3 * 3.49 * 10
-2(μ g/mL)=1.15 * 10
-1(μ g/mL)
6. linearity
Precision measures reference substance solution, by above-mentioned condition, detects, and result is as shown in table 7.
Table 7 sodion is linear
| Concentration (μ g/mL) | 0.5 | 1.0 | 1.5 | 2.0 | 2.5 |
| Absorbance (Abs) | 0.0679 | 0.1625 | 0.2722 | 0.3846 | 0.4942 |
Take absorbance (Abs) as ordinate (Y), and concentration (μ g/mL) is horizontal ordinate (X), calculates regression equation to be: Y=2.1494 * 10
-1 x-4.613 * 10
-2, r=0.9995.Illustrate that sodion is in the scope of 0.5 μ g/mL～2.5 μ g/mL, the linear relationship of concentration and absorbance is good.
Take absorbance (abs) as ordinate (Y), and the concentration of potassium ion is horizontal ordinate (X), and drawing standard curve, is shown in Fig. 2.
7. sample introduction precision
The sample that the lot number of take is 090401 (specification: 100mL: potassium chloride 0.11g and sodium chloride 0.9g) is test specimen, according to above-mentioned condition, tests, and METHOD FOR CONTINUOUS DETERMINATION 5 times, measurement result is in Table 8.
Table 8 Precision test result
| Measure number of times | 1 | 2 | 3 | 4 | 5 |
| Absorbance (Abs) | 0.3228 | 0.3229 | 0.3235 | 0.3220 | 0.3238 |
Same need testing solution replication 5 times, result mean value is 0.3230, relative standard deviation (RSD%) is 0.22%, meets mensuration requirement.
8. method reappearance
Get lot number and be 5 parts, 090401 sample (specification: 100mL: potassium chloride 0.11g and sodium chloride 0.9g), according to above-mentioned condition, test, measurement result is in Table 9.
Table 9 reproducible test results
| Numbering | 1 | 2 | 3 | 4 | 5 | 6 |
| Absorbance (Abs) | 0.3203 | 0.3293 | 03228 | 0.3222 | 0.3220 | 0.3196 |
Same lot number sample replication 5 times, result mean value is 0.3227, relative standard deviation (RSD%) is 1.07%, illustrates that this method reappearance is good.
9. test liquid stability
Lot number is that 090401 sample (specification: 100mL: potassium chloride 0.11g and sodium chloride 0.9g) is test specimen, according to above-mentioned condition, tests, and measures respectively at 0,1,2,4,8 hour, and measurement result is in Table 10.
Table 10 stability test result
| Time (h) | 0 | 1 | 2 | 4 | 8 |
| Absorbance (Abs) | 0.3206 | 0.3183 | 0.3221 | 0.3160 | 0.3218 |
Result mean value is 0.3198, and relative standard deviation (RSD%) is 0.807%, and the above results shows that need testing solution measured more stablely in 8 hours, can meet the needs of measuring.
10. the recovery:
Precision measures sodium standard solution (50 μ g/mL) 2.8mL, 3.6mL, 4.4mL, splits in 100mL measuring bottle, then precision measures blank test solution, and [potassium chloride 0.3g is dissolved in water and is diluted to 100mL, shakes up.Precision measures above-mentioned solution 5.0mL and puts in 100mL measuring bottle, is diluted with water to scale, shakes up] 1.0mL, be diluted with water to scale, shake up.By above-mentioned condition, detect, result is as shown in table 11.
Table 11: recovery test
| Numbering | Addition (μ g/mL) | Absorbance (Abs) | The amount of recording (μ g/mL) | The recovery (%) |
| 1 | 1.40 | 0.2533 | 1.3644 | 97.46 |
| 2 | 1.40 | 0.2545 | 1.3700 | 97.79 |
| 3 | 1.40 | 0.2551 | 1.3730 | 98.07 |
| 4 | 1.80 | 0.3298 | 1.7433 | 97.03 |
| 5 | 1.80 | 0.3305 | 1.7467 | 97.04 |
| 6 | 1.80 | 0.3294 | 1.7413 | 96.74 |
| 7 | 2.20 | 0.4254 | 2.2171 | 100.78 |
| 8 | 2.20 | 0.4248 | 2.2144 | 100.65 |
| 9 | 2.20 | 0.4183 | 2.1821 | 99.19 |
As seen from the above table, the recovery of nine test samples is between 96.74%～100.78%, and average recovery rate is that 98.32%, RSD is 1.57%, shows that this determination method can determine the content of sodion in sample exactly, and method is feasible.
The assay result of 11. 3 batch samples
Get test agent in three batches, by potassium chloride in sodium chloride inj content assaying method, measure, obtain on typical curve, finding corresponding concentration after absorbance, according to the concentration * extension rate/labelled amount of: content=check in, calculate content, it the results are shown in Table 12.
Sodium chloride content measurement result in table 12 sample
Therefore, according to this measurement result, in three batch samples of described three kinds of specifications, sodium chloride (NaCl) content is labelled amount 96.02～101.24%, up to specification 95.0～105.0%.
Claims (8)
1. an assay method for the KCE content of potassium chloride in sodium chloride inj, described method adopts atomic absorption spectrophotometer (AAS) to be undertaken by atomic absorption spectrophotometry, it is characterized in that, said method comprising the steps of:
1) preparation of blank test solution:
By 0.7g～1.1g sodium chloride, preferred 0.8～1.0g sodium chloride, more preferably 0.9g sodium chloride is dissolved in water and is diluted to 100mL, shakes up, and precision measures gained solution 5.0mL, is placed in 50mL measuring bottle, is diluted with water to scale, shakes up, and obtains blank test solution;
2) preparation of reference substance solution:
Precision measures the potassium standard solution 5.0mL that concentration is 1000 μ g/mL, be placed in 50mL measuring bottle, be diluted with water to scale, shake up, obtain the solution that concentration is 100 μ g/mL, precision measures solution 1.0mL, 2.0mL, 3.0mL, 4.0mL and the 5.0mL of 100 μ g/mL, be placed in respectively 100mL measuring bottle, then precision adds blank test solution 5.0mL, be diluted with water to scale, shake up, obtain reference substance solution;
3) preparation of need testing solution:
Precision measures testing sample, and thin up is made the potassium ion solution that concentration is about 3 μ g/mL, obtains need testing solution;
4) measure:
Adopt the absorbance of atomic absorption spectrophotometry detection reference substance solution, drawing standard curve; Detect the absorbance of need testing solution, calculate content.
2. the method for claim 1, is wherein used resistivity for the ultrapure water of 18M Ω CM.
3. method as claimed in claim 1 or 2, wherein, the setup parameter of described atomic absorption spectrophotometer (AAS) is:
Lamp current: 7～12mA, is preferably 12.0mA;
Slit: 1.3nm or 0.4nm, be preferably 1.3nm;
Wavelength: 766.5nm; And
Burner height: 5～10mm, is preferably 7.5mm.
4. an assay method for the sodium chloride content of potassium chloride in sodium chloride inj, described method adopts atomic absorption spectrophotometer (AAS) to be undertaken by atomic absorption spectrophotometry, it is characterized in that, said method comprising the steps of:
1) preparation of blank test solution:
By 0.1g～0.5g potassium chloride, preferred 0.2～0.4g potassium chloride, more preferably 0.3g potassium chloride is dissolved in water and is diluted to 100mL, shakes up, and precision measures gained solution 5.0mL, is placed in 100mL measuring bottle, is diluted with water to scale, shakes up, and obtains blank test solution;
2) preparation of reference substance solution:
Precision measures the sodium standard solution 5.0mL that concentration is 1000 μ g/mL, be placed in 100mL measuring bottle, be diluted with water to scale, shake up, obtain the solution that concentration is 50 μ g/mL, precision measures solution 1.0mL, 2.0mL, 3.0mL, 4.0mL and the 5.0mL of 50 μ g/mL, be placed in respectively 100mL measuring bottle, then precision adds blank test solution 1.0mL, be diluted with water to scale, shake up, obtain reference substance solution;
3) preparation of need testing solution:
Precision measures testing sample, and thin up is made the sodion solution that concentration is about 1.8 μ g/mL, obtains need testing solution;
4) measure:
Adopt the absorbance of atomic absorption spectrophotometry detection reference substance solution, drawing standard curve; Detect the absorbance of need testing solution, calculate content.
5. method as claimed in claim 4, is wherein used resistivity for the ultrapure water of 18M Ω CM.
6. the method as described in claim 4 or 5, wherein, the setup parameter of described atomic absorption spectrophotometer (AAS) is:
Lamp current: 8～12mA, is preferably 12.0mA;
Slit: 0.4nm or 1.3nm, be preferably 0.4nm;
Wavelength: 589.0nm; And
Burner height: 5～10mm, is preferably 7.5mm.
7. whether the KCE content of a definite potassium chloride in sodium chloride inj meets the method for quality standard, it is characterized in that, method in employing claim 1～3 described in any one is measured the KCE content of potassium chloride in sodium chloride inj and/or is adopted the sodium chloride content of the mensuration of the method described in any one potassium chloride in sodium chloride inj in claim 4～6, if to measure the KCE content obtain and/or sodium chloride content be labelled amount 95.0%～105.0%, this potassium chloride in sodium chloride inj meets quality standard.
8. the method as described in claim 1～7 any one, for the mensuration of following potassium chloride in sodium chloride inj potassium chloride or sodium chloride content:
(1) 100mL: the potassium chloride in sodium chloride inj of potassium chloride 0.11g and sodium chloride 0.9g;
(2) 100mL: the potassium chloride in sodium chloride inj of potassium chloride 0.22g and sodium chloride 0.9g;
(3) 100mL: the potassium chloride in sodium chloride inj of potassium chloride 0.11g and sodium chloride 0.9g.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104964939A (en) * | 2015-06-30 | 2015-10-07 | 山东丹红制药有限公司 | Method for detecting content of sodium and potassium ions in Danhong injection |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1326448A (en) * | 1970-06-03 | 1973-08-15 | Hitachi Ltd | Atomic absorption photometer |
| CN101398373A (en) * | 2007-09-26 | 2009-04-01 | 比亚迪股份有限公司 | Method for detecting potassium and/or sodium content in soluble lithium compounds |
| CN101566561A (en) * | 2009-05-26 | 2009-10-28 | 上海大学 | Method for measuring microelement in radish |
| CN101571478A (en) * | 2009-06-15 | 2009-11-04 | 株洲硬质合金集团有限公司 | Method for analyzing and detecting potassium and sodium impurity elements in vanadium carbide |
| CN102526098A (en) * | 2010-12-08 | 2012-07-04 | 四川奇力制药有限公司 | New application of compound sodium chloride potassium chloride injection |
-
2012
- 2012-08-08 CN CN201210280764.1A patent/CN103575669B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1326448A (en) * | 1970-06-03 | 1973-08-15 | Hitachi Ltd | Atomic absorption photometer |
| CN101398373A (en) * | 2007-09-26 | 2009-04-01 | 比亚迪股份有限公司 | Method for detecting potassium and/or sodium content in soluble lithium compounds |
| CN101566561A (en) * | 2009-05-26 | 2009-10-28 | 上海大学 | Method for measuring microelement in radish |
| CN101571478A (en) * | 2009-06-15 | 2009-11-04 | 株洲硬质合金集团有限公司 | Method for analyzing and detecting potassium and sodium impurity elements in vanadium carbide |
| CN102526098A (en) * | 2010-12-08 | 2012-07-04 | 四川奇力制药有限公司 | New application of compound sodium chloride potassium chloride injection |
Non-Patent Citations (4)
| Title |
|---|
| 全英花等: "火焰光度法测定复方氯化钠注射液中氯化钾含量", 《中国药品标准》 * |
| 匡洪红等: "火焰原子吸收法测定氯化钾产品中钠离子含量", 《盐业与化工》 * |
| 林洪等: "原子吸收光谱法测定复方氯化钠注射液中氯化钾的含量", 《山东医药工业》 * |
| 林洪等: "原子吸收光谱法测定复方氯化钠注射液中氯化钾的含量", 《山东医药工业》, vol. 18, no. 3, 31 December 1999 (1999-12-31) * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104964939A (en) * | 2015-06-30 | 2015-10-07 | 山东丹红制药有限公司 | Method for detecting content of sodium and potassium ions in Danhong injection |
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