CN104964939A - Method for detecting content of sodium and potassium ions in Danhong injection - Google Patents
Method for detecting content of sodium and potassium ions in Danhong injection Download PDFInfo
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Abstract
The invention provides a method for detecting the content of sodium and potassium ions in a Danhong injection. A microwave digestion system is used for digesting a sample, and the sodium and potassium ions are detected at 589.0nm and 766.9nm parts by a flame atomic absorption spectrophotometric method; systematic methodological evaluation is carried out and a result shows that the sodium ions have a good linear relation in a range of 0.1 to 0.6 microgram/mL, and the potassium ions have a good linear relation in a range of 0.1 to 0.8 microgram/mL. The method has good recycling rate and repeatability, and meets the requirements of content determination. The method for determining the content of the sodium and potassium ions is simple to operate and feasible, has an accurate and reliable result, can be used for determining the content of the sodium and potassium ions in the Danhong injection and is applied to quality control researches of the Danhong injection.
Description
Technical field
The invention belongs to the technical field that in traditional Chinese medicine injection, metallic ion measures, particularly relate to the detection method of content of sodium, potassium ion in a kind of DANHONG ZHUSHEYE, can be used as the quality controling research of DANHONG ZHUSHEYE.
Background technology
DANHONG ZHUSHEYE is prepared from through modern pharmaceutical technique by the red sage root 750 parts, 250 parts, safflower, and wherein the red sage root is monarch drug in a prescription, and safflower is ministerial drug.DANHONG ZHUSHEYE has promoting blood circulation and removing blood stasis; promoting blood circulation, activating collaterals, eliminating phlegm to promote tissue regeneration, evil removing does not hinder positive effect; to the capillary endothelium of anoxia-induced apoptosis, there is protective effect, be used for the treatment of the disease such as the obstruction of qi in the chest and apoplexy, coronary heart diseases and angina pectoris, miocardial infarction caused by hemostasis impatency clinically.
Version " Chinese Pharmacopoeia " regulation in 2010: the quality check of injection liquid in use for intravenous injection all requires the limit test carrying out potassium ion.Sodium, potassium are the electrolyte in body, the too high or too low dysfunction that all can cause N&M of blood potassium, severe person can occur ventricular fibrillation, drowsiness, even go into a coma, sudden arrest of heart beat; The too high or too low brain cell that makes of blood sodium dewaters or oedema, threat to life.In traditional Chinese medicine, potassium content is too high, obvious local excitation (pain reaction) and cardiac damage can be caused, during for intravenous injection, Blood of Patients potassium concentration can be caused higher, make electrolyte disturbance, therefore tackle potassium ion in injection used for intravenous injection and carry out limit examine.
In view of recent traditional Chinese medicine injection bad reaction takes place frequently, sodium in traditional Chinese medicine injection, the content of potassium ion are one of influence factors producing bad reaction, and also not yet carry out the content detection of sodium in DANHONG ZHUSHEYE, potassium ion at present, therefore the present invention sets up the content that atomic absorption spectrophotometry measures sodium, potassium ion, seems particularly important.Therefore, the present invention adopts atomic absorption spectrophotometry, carries out assay to sodium, potassium ion in DANHONG ZHUSHEYE, more fully to control and to reflect the quality of DANHONG ZHUSHEYE, ensures security and the validity of DANHONG ZHUSHEYE clinical application.
Summary of the invention
Technical matters to be solved by this invention sets up the content assaying method of sodium, potassium ion in a kind of DANHONG ZHUSHEYE, and the method is easy, quick, accurate, for controlling DANHONG ZHUSHEYE quality, instructs data for clinical drug use to provide experiment basis.
In the DANHONG ZHUSHEYE that the present invention adopts, the technical scheme of sodium, potassium content assay method is: the present invention adopts atomic absorption spectrophotometry to measure, and the method comprises the steps:
(1) the preparation of blank solution:
Weigh 0.5 ~ 1.5g cesium chloride, be placed in 100mL measuring bottle, be dissolved in water and be settled to scale, for subsequent use as ionization buffer, get 1mL ionization buffer and be placed in 10mL measuring bottle, then be diluted to scale with ultrapure water, shake up, to obtain final product;
(2) the preparation of need testing solution:
Get DANHONG ZHUSHEYE 0.1 ~ 0.3mL and be placed in counteracting tank, add red fuming nitric acid (RFNA) 4mL, 8 ~ 12min time-to-climb of in microwave dissolver, clear up 25 ~ 35min in 180 ~ 220 DEG C, after cooling, take out observation, solution clear, without insolubles, digestion solution is heated near dry, adds dilution (ultrapure water), be transferred to 50mL measuring bottle, wash counteracting tank with dilution, and be progressively transferred to measuring bottle, add dilution to scale, shake up, as sodium/potassium ion test sample stock solution; Get test sample stock solution 2 ~ 4mL, add ionization buffer 1 ~ 5mL, then be diluted to 10 ~ 50mL with ultrapure water, shake up, as sodium/potassium ion need testing solution;
(3) the preparation of sodium/potassium ion reference substance solution:
Precision measures sodium/potassium ion standard solution, is placed in measuring bottle, is diluted with water to scale, shake up, and obtains ion standard working solution; Get ion standard working solution to put in right amount in measuring bottle, add ionization buffer respectively, then dilute scale with ultrapure water, shake up, as sodium/potassium ion reference substance solution, use for drawing standard curve;
(4) assay:
Atomic absorption spectrophotometry is adopted to detect the absorbance of reference substance solution, drawing standard curve; And detect the absorbance of need testing solution, calculate content.
As preferably of the present invention, the preparation process of described detection method step (1) empty solution is, weigh 1.0g cesium chloride, be placed in 100mL measuring bottle, be dissolved in water and be settled to scale, for subsequent use as ionization buffer, get 1mL ionization buffer and be placed in 10mL measuring bottle, be diluted to scale with ultrapure water again, shake up, to obtain final product.
As preferably of the present invention, described detection method step (2) in the preparation process of need testing solution be, get DANHONG ZHUSHEYE 0.2mL and be placed in counteracting tank, add 4mL red fuming nitric acid (RFNA), the 10min time-to-climb of in microwave dissolver, clears up 30min in 200 DEG C, takes out observation after cooling, solution clear, without insolubles, digestion solution is heated near dry, adds ultrapure water dilution, be transferred to 50mL measuring bottle, wash counteracting tank with dilution, and be progressively transferred to measuring bottle, add dilution to scale, shake up, as sodium/potassium ion test sample stock solution; Get test sample stock solution 2 ~ 4mL, add ionization buffer 1 ~ 5mL, then be diluted to 10 ~ 50mL with ultrapure water, shake up, as sodium/potassium ion need testing solution.
As preferably of the present invention, described detection method step (3) in the preparation process of reference substance sodium/potassium solution: precision measures sodium/potassium ion standard solution, is placed in measuring bottle, is diluted with water to scale, shake up, and obtaining concentration is 10 μ gmL
-1ion standard working solution; Get sodium/potassium ion standard working solution appropriate, add ionization buffer respectively, ultrapure water is diluted to measuring bottle scale, shakes up, as sodium/potassium ion reference substance solution.
As preferably of the present invention, the detection method of sodium/potassium content in the DANHONG ZHUSHEYE of foundation, the method comprises the steps:
(1) the preparation of blank solution:
Weigh 1.0g cesium chloride, be placed in 100mL measuring bottle, be dissolved in water and be settled to scale, for subsequent use as ionization buffer, get 1mL ionization buffer and be placed in 10mL measuring bottle, then be diluted to scale with ultrapure water, shake up, to obtain final product;
(2) the preparation of need testing solution:
Get DANHONG ZHUSHEYE 0.2mL and be placed in counteracting tank, add 4mL red fuming nitric acid (RFNA), the 10min time-to-climb of in microwave dissolver, clear up 30min in 200 DEG C, after cooling, take out observation, solution clear, without insolubles, digestion solution is heated near dry, adds ultrapure water dilution, be transferred to 50mL measuring bottle, wash counteracting tank with dilution, and be progressively transferred to measuring bottle, add dilution to scale, shake up, as sodium/potassium ion test sample stock solution.
Get test sample stock solution 3.125mL to put in 50mL measuring bottle, add 5mL ionization buffer, ultrapure water is diluted to scale, shakes up, as sodion need testing solution;
Get test sample stock solution 2mL to put in 10mL measuring bottle, add 1mL ionization buffer, ultrapure water is diluted to scale, shakes up, as potassium ion need testing solution;
(3) the preparation of sodium/potassium ion reference substance solution:
Precision measures sodium/potassium ion standard solution (1000 μ gmL
-1) appropriate, be placed in measuring bottle, be diluted with water to scale, shake up, obtaining concentration is 10 μ gmL
-1ion standard working solution; Get sodium/potassium ion standard working solution appropriate, add ionization buffer respectively, ultrapure water is diluted to measuring bottle scale, shakes up, as sodium/potassium ion reference substance solution;
(4) assay:
Atomic absorption spectrophotometry is adopted to detect the absorbance of reference substance solution, drawing standard curve; And detect the absorbance of need testing solution, calculate content.
Sodium ions content detection method in the DANHONG ZHUSHEYE that the present invention sets up, the condition of work of Atomic Absorption Spectrometer is as follows: measure wavelength: 589.0nm, sodium spectrum bandwidth: 2nm, lamp current: 2mA, negative high voltage (-V): 300, gas flow 1.1Lmin
-1, burner height: 5.0nm; Adopt air-acetylene flame.
Potassium content detection method in the DANHONG ZHUSHEYE that the present invention sets up, use the condition of work of Atomic Absorption Spectrometer as follows: to measure wavelength: 766.9nm, potassium spectral bandwidth: 2nm, lamp current: 2mA, negative high voltage (-V): 300, gas flow: 1.7Lmin
-1, burner height: 5.0nm; Adopt air-acetylene flame.
The detection method that the present invention sets up can be used for the detection of DANHONG ZHUSHEYE sodium/potassium content.
Beneficial effect of the present invention:
(1) the present invention adopts and adds the lower cesium chloride of ionization potential as ionization inhibitor, and eliminate ionization interference, can improve measurement sensistivity, wherein the concentration limit of sodion is 5.3ngmL simultaneously
-1, the concentration limit of potassium ion is 7.7ngmL
-1.
(2) the present invention adopts microwave digestion technology in sample preparation, the method have clear up sample heating fast, heat up high, ability of clearing up is strong, substantially reduce molten sample time, non-environmental-pollution and reduce the advantages such as energy dissipation.Because DANHONG ZHUSHEYE sample itself is aqueous solution, adopt the method processing sample recovery of directly dilution low, do not meet methodological study requirement, the mensuration of interpret sample matrix to sodium, potassium ion has interference, therefore adopt micro-wave digestion process, sample substrate after clearing up is very little to the absorption of sodium, potassium ion interference, can sodium, potassium content in Accurate Determining DANHONG ZHUSHEYE.
(3) the atomic absorption spectrophotometry that the present invention sets up measures the method for sodium, potassium content in DANHONG ZHUSHEYE, operation is simple and feasible, result accurately and reliably, the recovery is high, linear relationship is good within the specific limits, and reproducible, the content of sodium in DANHONG ZHUSHEYE, potassium ion can be measured fast, can be used for the quality controling research of DANHONG ZHUSHEYE.
According to 2010 version " Chinese Pharmacopoeia " annex " parenteral solution Related substances separation method " research require: adopt colourimetry carry out potassium ion limit examine in need testing solution, require that need testing solution color must not than potassium ion solution (100 μ gmL
-1) color is darker, therefore converting parenteral solution potassium content must not more than 1000 μ gmL
-1.By to 10 batches of DANHONG ZHUSHEYE sample tests, actual measured value does not all exceed specialized range, meets pharmacopeia relevant regulations.The average of DANHONG ZHUSHEYE is about 30mgmL containing thing amount admittedly
-1the content calculating sodion accounts for DANHONG ZHUSHEYE always admittedly containing 1.9 ~ 2.4% of thing, the content of potassium ion accounts for DANHONG ZHUSHEYE always admittedly containing 0.7 ~ 1.0% of thing, sodium, potassium ion total amount account for DANHONG ZHUSHEYE always admittedly containing 2.6 ~ 3.4% of thing, provide experimental data for instructing data for clinical drug use.
(5) in existing bibliographical information, the normal Sodium Tetraphenylborate Method that adopts measures potassium concentration, and the method exists trivial operations and time-consuming shortcoming; Sodion measures and adopts ICP-AES method etc., but there is the shortcoming that analysis cost is high, not easily promote.Compared with the method, method of the present invention have detect easy, accuracy is high, lower-cost advantage.
Accompanying drawing explanation
Fig. 1 is sodion canonical plotting.
Fig. 2 is potassium ion canonical plotting.
Embodiment
In order to make those skilled in the art better understand technical scheme of the present invention, below in conjunction with the drawings and the specific embodiments, technical scheme of the present invention is described in further detail.
Be used for the present invention is described by case study on implementation below, but be not used for limiting the scope of the invention.One of skill in the art can understand, and under the prerequisite not deviating from the spirit and scope of the present invention, can carry out various change and modification to the present invention.The present invention carries out generality or concrete description to the material used in test and test method.Although for realizing many materials that the object of the invention uses and method of operating is well known in the art, the present invention still describes in detail as far as possible at this.In the present invention, as not dated especially, detect use sample to be DANHONG ZHUSHEYE, and with Absorbance versus concentration (μ gmL
-1) make curve, obtain standard working curve, calculate the concentration of sodium in need testing solution, potassium ion with external standard method.DANHONG ZHUSHEYE sample is provided by Shandong Dan Hong pharmaceutical Co. Ltd, methodological study sample lot number: 13081025.
Embodiment 1: atomic absorption spectrophotometry measures the content of sodion in DANHONG ZHUSHEYE.
1.1 instruments and reagent
TAS-990 atomic absorption spectrophotometer (AAS) (Beijing Puxi General Instrument Co., Ltd); Sodium hollow cathode lamp (Beijing Shuguangming Electronic Lighting Instrument Co., Ltd.); Flame burner (Beijing Puxi General Instrument Co., Ltd).
Analytical reagent: sodium (Na) single element standard solution (national non-ferrous metal and electronic material Institute of Analysis, unique identification 11042, concentration 1000 μ gmL
-1, medium 5%HCl).Cesium chloride (lot number 20090825, Tianjin Jin Ke fine chemistry industry research institute), ultrapure water (self-control of Milli-Q pure water instrument), nitric acid (top grade is pure, Beijing Chemical Plant).Experiment DANHONG ZHUSHEYE is commercially available prod, specification is for often propping up dress 10mL, Shandong Dan Hong pharmaceutical Co. Ltd of manufacturer, 10 batch sample lot numbers are respectively 14031035,14041013,14051016,14051008,14061001,14071047,14041035,14081005,14081007,14081003.
The preparation of 1.2 blank solutions:
Weigh 1g cesium chloride, be placed in 100mL measuring bottle, be dissolved in water and be settled to scale, as ionization buffer, get 1mL ionization buffer to 10mL measuring bottle, then be diluted to scale with ultrapure water, shake up, to obtain final product.
The preparation of 1.3 need testing solutions:
Get 0.2mL sample and be placed in counteracting tank, add 4mL red fuming nitric acid (RFNA), the 10min time-to-climb of in microwave dissolver, clear up 30min for 200 DEG C.Observation is taken out after cooling, solution clear, without insolubles, digestion solution is heated near dry, adds dilution (ultrapure water) 10mL, be transferred to 50mL measuring bottle, wash counteracting tank with dilution, and be transferred to measuring bottle gradually, add dilution to scale, shake up, as sodion test sample stock solution; Get test sample stock solution 3.125mL to put in 50mL measuring bottle, add 5mL ionization buffer, then be diluted to scale with ultrapure water, shake up, as sodion need testing solution.
The preparation of 1.4 sodion reference substance solution:
Precision measures sodium metal ion standard solution (1000 μ gmL
-1) 0.5mL, be placed in 50mL measuring bottle, be diluted with water to scale, shake up, obtaining concentration is 10 μ gmL
-1sodion standard working solution.
1.5 assays:
The detection method of described mensuration sodium ions content, uses the condition of work of Atomic Absorption Spectrometer as follows: to measure wavelength: 589.0nm, sodium spectrum bandwidth: 2nm, lamp current: 2mA, negative high voltage (-V): 300, gas flow 1.1Lmin
-1, burner height: 5.0nm; Adopt air-acetylene flame.
1.5.1 the drafting of typical curve
Precision measures sodion standard working solution 0.1,0.2,0.4,0.5,0.6mL under above-mentioned " 1.4 ", is placed in 10mL measuring bottle respectively, adds ionization buffer 1mL respectively, add ultrapure water and be diluted to scale, obtain concentration and be respectively 0.1,0.2,0.4,0.5,0.6 μ gmL
-1solution as working curve solution, sequentially determining absorbance take absorbency Y as ordinate, concentration X (μ gmL
-1) be horizontal ordinate, drawing standard curve.Obtain regression equation: A=0.6243C+0.0037, correlation coefficient r=0.9998, show that sodion is at 0.1 ~ 0.6 μ gmL
-1with absorbance, there is good linear relationship in scope.
1.5.2 the mensuration of detection limit
Get blank solution, METHOD FOR CONTINUOUS DETERMINATION 11 absorbances, obtain its standard deviation, calculate detection limit (C according to the following formula
l).
According to C
l(μ gmL
-1)=3S
a/ S, wherein, S
a: blank solution standard deviation; S: standard working curve slope.
Result shows, blank solution measures for continuous 11 times, absorbance is respectively: 0.015,0.014,0.013,0.015,0.014,0.012,0.012,0.014,0.015,0.014,0.014, standard deviation is 0.0011, according to the slope in equation of linear regression, the concentration limit calculating sodion is 5.3ngmL
-1.
1.5.3 precision test
Get 0.4 μ gmL
-1reference substance solution, direct injected, measure absorbances continuous seven times, calculate RSD value, result RSD is 1.0%, shows that instrument performance is stable.(table 1)
Table 1 sodion Precision test result
1.5.4 replica test
Get 0.2mL sample and be placed in counteracting tank, add 4mL red fuming nitric acid (RFNA), clear up sample by the preparation method of need testing solution under " 1.3 ", parallelly clear up six parts, digestion solution is heated near dry, is progressively transferred to 50mL measuring bottle with dilution washing counteracting tank, adds dilution to scale; Precision measures 3.125mL and puts in 50mL measuring bottle, adds 5mL ionization buffer, and ultrapure water dilutes and is settled to scale, shake up, parallel preparation 6 parts of need testing solutions, measure, RSD is 1.0%, shows that the method measures the repeatability good (the results are shown in Table 2) of DANHONG ZHUSHEYE sodion.
Table 2 sodion replica test result
1.5.5 recovery test
Get 0.1mL sample and be placed in counteracting tank, add 80 μ L 1000 μ gmL
-1sodion titer, then add 4mL red fuming nitric acid (RFNA), clear up sample by the preparation method of need testing solution under " 1.3 ", parallelly clear up six parts, digestion solution is heated near dry, be progressively transferred to 50mL measuring bottle with dilution washing counteracting tank, add dilution to scale, shake up; Precision measures 3.125mL and puts in 50mL measuring bottle, adds 5mL ionization buffer, and ultrapure water dilutes and is settled to scale, shakes up, respectively the absorbance of working sample, calculates the recovery of sodion.Result shows, the recovery of this detection method is good, meets to measure to require (the results are shown in Table 3).
Table 3 sodion recovery test result
1.5.6 the stability test of sodion in need testing solution
Get need testing solution portion, preserve under room temperature, measure its absorbance log respectively at 0h, 1h, 2h, 4h, 6h, investigate the stability of sodion in need testing solution, result to show in need testing solution that sodion is in room temperature preservation 6 hours stable (the results are shown in Table 4).
Sodion stability test result in table 4 need testing solution
1.5.7 the assay of sample
Adopt the assay method of the sodion of above-mentioned foundation, sodion in 10 batches of DANHONG ZHUSHEYEs is measured, the results are shown in Table 5.
Measurement result (the μ gmL of sodion in table 5 10 batches of DANHONG ZHUSHEYE samples
-1)
Embodiment 2, atomic absorption spectrophotometry measure the content of potassium ion in DANHONG ZHUSHEYE.
2.1 instruments and reagent
TAS-990 atomic absorption spectrophotometer (AAS) (Beijing Puxi General Instrument Co., Ltd); Potassium hollow cathode lamp (Beijing Shuguangming Electronic Lighting Instrument Co., Ltd.); Flame burner (Beijing Puxi General Instrument Co., Ltd).
Analytical reagent: potassium (K) single element standard solution (national non-ferrous metal and electronic material Institute of Analysis, unique identification 12303-2, concentration 1000 μ gmL
-1, medium H
2o), cesium chloride (lot number 20090825, Tianjin Jin Ke fine chemistry industry research institute), ultrapure water (self-control of Milli-Q pure water instrument), nitric acid (top grade is pure, Beijing Chemical Plant).Experiment DANHONG ZHUSHEYE is commercially available prod, specification is for often propping up dress 10mL, Shandong Dan Hong pharmaceutical Co. Ltd of manufacturer, 10 batch sample lot numbers are respectively 14031035,14041013,14051016,14051008,14061001,14071047,14041035,14081005,14081007,14081003.
The preparation of 2.2 blank solutions:
Weigh 1g cesium chloride, be placed in 100mL measuring bottle, be dissolved in water and be settled to scale, for subsequent use as ionization buffer, get 1mL ionization buffer and be placed in 10mL measuring bottle, ultrapure water is diluted to scale, shakes up, and to obtain final product.
The preparation of 2.3 need testing solutions:
Get 0.2mL sample and be placed in counteracting tank, add 4mL red fuming nitric acid (RFNA), the 10min time-to-climb of in microwave dissolver, clear up 30min for 200 DEG C.Take out observation after cooling, solution clear, without insolubles, digestion solution is heated near dry, add dilution 10mL, be transferred in 50mL measuring bottle, with ultrapure water dilution washing counteracting tank, and be transferred to measuring bottle gradually, add dilution to scale, shake up, as test sample stock solution; Get test sample stock solution 2mL to put in 10mL measuring bottle, add 1mL ionization buffer, ultrapure water is settled to scale, shakes up, as potassium ion need testing solution.
The preparation of 2.4 potassium ion reference substance solution:
Precision measures metallic potassium ion standard solution (1000 μ gmL
-1) 0.5mL, be placed in 50mL measuring bottle, add ultrapure water and be diluted to scale, shake up, obtaining concentration is 10 μ gmL
-1potassium ion standard working solution.
2.5 assays:
Method: the condition of work of atomic absorption spectrophotometer (AAS) is for measuring wavelength: 766.9nm, potassium spectral bandwidth: 2nm, lamp current: 2mA, negative high voltage (-V): 300, potassium gas flow: 1.7Lmin-1, burner height: 5.0nm; Adopt air-acetylene flame.
2.5.1 the drafting of typical curve
Precision measures potassium ion standard working solution 0.1,0.2,0.4,0.6,0.8mL under above-mentioned " 2.4 ", and be placed in 10mL measuring bottle respectively, add ionization buffer 1mL respectively, ultrapure water is diluted to scale, obtains concentration and is respectively 0.1,0.2,0.4,0.6,0.8 μ gmL
-1solution as working curve solution, measure, take absorbency Y as ordinate in accordance with the law, concentration X (μ gmL
-1) be horizontal ordinate, drawing standard curve.Obtain regression equation: A=0.4348C+0.0072, correlation coefficient r=0.9998, show that potassium ion is at 0.1 ~ 0.8 μ gmL
-1with absorbance, there is good linear relationship in scope.As Fig. 2.
2.5.2 the mensuration of potassium ion detection limit
Get blank solution, METHOD FOR CONTINUOUS DETERMINATION 11 absorbances, ask its standard deviation, calculate detection limit (C according to the following formula
l).
According to C
l(μ gmL
-1)=3S
a/ S, wherein, S
a: blank solution standard deviation; S: standard working curve slope.
Result shows, blank solution measures for continuous 11 times, absorbance is respectively: 0.011,0.010,0.010,0.008,0.008,0.008,0.008,0.008,0.008,0.008,0.008, standard deviation is 0.0011, according to the slope in equation of linear regression, the concentration limit calculating potassium ion is 7.7ngmL
-1.
2.5.3 precision test
Get 0.2 μ gmL
-1reference substance solution, direct injected, measures absorbances, calculates RSD value for continuous seven times.Result RSD is 0.7%, shows that instrument performance is stablized.(the results are shown in Table 6).
Table 6 potassium ion Precision test result
2.5.4 replica test
Get 0.2mL sample and be placed in counteracting tank, add 4mL red fuming nitric acid (RFNA), clear up sample by the preparation method of need testing solution under " 2.3 ", parallelly clear up six parts, digestion solution is heated near dry, be progressively transferred in 50mL measuring bottle with dilution washing counteracting tank, add dilution to scale, shake up; Precision measures 2mL and puts 10mL measuring bottle, adds 1mL ionization buffer, and ultrapure water dilutes and is settled to scale, shake up, parallel preparation 6 parts of need testing solutions, measure respectively, RSD is 0.7%, shows that the method measures the repeatability good (the results are shown in Table 7) of DANHONG ZHUSHEYE potassium content.
Table 7 potassium ion replica test result
2.5.5 recovery test
Get 0.1mL sample and be placed in counteracting tank, add 25 μ L, 1000 μ gmL
-1potassium ion titer, add 4mL red fuming nitric acid (RFNA) again, sample is cleared up by the preparation method of need testing solution under " 2.3 ", parallelly clear up six parts, digestion solution is heated near dry, is also progressively transferred in 50mL measuring bottle with dilution washing counteracting tank, adds dilution to scale, shake up, as test sample stock solution; Precision measures 2mL and puts in 10mL measuring bottle, adds 1mL ionization buffer, and ultrapure water dilutes and is settled to scale, shakes up, respectively the potassium concentration of working sample, calculates the recovery of potassium ion.Result shows, the recovery of this detection method is good, meets to measure to require (the results are shown in Table 8).
Table 8 potassium ion recovery test result
2.5.6 the stability test of potassium ion in need testing solution
Get need testing solution portion, preserve under room temperature, measure its absorbance log respectively at 0h, 1h, 2h, 4h, 6h, investigate the stability of need testing solution potassium ion, result shows, need testing solution potassium ion is stable (the results are shown in Table 9) in room temperature preservation 6 hours.
Potassium ion stability test result in table 9 need testing solution
2.5.7 the assay of sample
Adopt the assay method of the potassium ion of above-mentioned foundation, potassium ion in 10 batches of DANHONG ZHUSHEYEs is measured, the results are shown in Table 10.
Measurement result (the μ gmL of potassium ion in table 10 10 batches of DANHONG ZHUSHEYE samples
-1)
From the measurement result of above-mentioned 10 batches of DANHONG ZHUSHEYE sample sodium/potassium ions, in DANHONG ZHUSHEYE, the content range of sodion is 562.3 ~ 734.7 μ gmL
-1, potassium content scope is at 206.9 ~ 314.4 μ gmL
-1.
In sum, show that the detection method of sodium that the present invention sets up, potassium ion is simple to operate fast, result accurately and reliably, reproducible, be applicable to the detection of sodium in DANHONG ZHUSHEYE, potassium ion, can be used for the research of DANHONG ZHUSHEYE quality control.
Claims (7)
1. the detection method of sodium/potassium content in DANHONG ZHUSHEYE, described detection method adopts atomic absorption spectrophotometry to measure, and it is characterized in that, described method comprises the steps:
(1) the preparation of blank solution:
Weigh 0.5 ~ 1.5g cesium chloride, be placed in 100mL measuring bottle, be dissolved in water and be settled to scale, for subsequent use as ionization buffer, get 1mL ionization buffer and be placed in 10mL measuring bottle, then be diluted to scale with ultrapure water, shake up, to obtain final product;
(2) the preparation of need testing solution:
Get DANHONG ZHUSHEYE 0.1 ~ 0.3mL and be placed in counteracting tank, add red fuming nitric acid (RFNA) 4mL, 8 ~ 12min time-to-climb of in microwave dissolver, clear up 25 ~ 35min in 180 ~ 220 DEG C, after cooling, take out observation, solution clear, without insolubles, digestion solution is heated near dry, adds ultrapure water dilution, be transferred to 50mL measuring bottle, wash counteracting tank with dilution, and be progressively transferred to measuring bottle, add dilution to scale, shake up, as sodium/potassium ion test sample stock solution; Get test sample stock solution 2 ~ 4mL, add ionization buffer 1 ~ 5mL, then be diluted to 10 ~ 50mL with ultrapure water, shake up, as sodium/potassium ion need testing solution;
(3) the preparation of sodium/potassium ion reference substance solution:
Precision measures sodium/potassium ion standard solution, is placed in measuring bottle, is diluted with water to scale, shake up, and obtains ion standard working solution; Getting ion standard working solution puts in measuring bottle, adds ionization buffer respectively, then is diluted to scale with ultrapure water, shake up, as sodium/potassium ion reference substance solution;
(4) assay:
Atomic absorption spectrophotometry is adopted to detect the absorbance of reference substance solution, drawing standard curve; And detect the absorbance of need testing solution, calculate content.
2. the as described in claim 1 detection method of sodium/potassium content in DANHONG ZHUSHEYE, it is characterized in that, the preparation process of described detection method step (1) empty solution is, weighs 1.0g cesium chloride, is placed in 100mL measuring bottle, be dissolved in water and be settled to scale, for subsequent use as ionization buffer, get 1mL ionization buffer and be placed in 10mL measuring bottle, then be diluted to scale with ultrapure water, shake up, to obtain final product.
3. the as described in claim 1 detection method of sodium/potassium content in DANHONG ZHUSHEYE, it is characterized in that, described detection method step (2) in the preparation process of need testing solution be, get DANHONG ZHUSHEYE 0.2mL and be placed in counteracting tank, add 4mL red fuming nitric acid (RFNA), the 10min time-to-climb of in microwave dissolver, 30min is cleared up in 200 DEG C, observation is taken out after cooling, solution clear, without insolubles, digestion solution is heated near dry, add ultrapure water dilution, be transferred to 50mL measuring bottle, counteracting tank is washed with dilution, and be progressively transferred to measuring bottle, add dilution to scale, shake up, as sodium/potassium ion test sample stock solution, get test sample stock solution 2 ~ 4mL, add ionization buffer 1 ~ 5mL, then be diluted to 10 ~ 50mL with ultrapure water, shake up, as sodium/potassium ion need testing solution.
4. the as described in claim 1 detection method of sodium/potassium content in DANHONG ZHUSHEYE, it is characterized in that, described detection method step (3) in the preparation process of reference substance sodium/potassium ion solution be: precision measures sodium/potassium ion standard solution, be placed in measuring bottle, be diluted with water to scale, shake up, obtaining concentration is 10 μ gmL
-1ion standard working solution; Get sodium/potassium ion standard working solution, add ionization buffer respectively, ultrapure water is diluted to measuring bottle scale, shakes up, as sodium/potassium ion reference substance solution.
5. the as described in claim 1 detection method of sodium/potassium content in DANHONG ZHUSHEYE, it is characterized in that, described detection method comprises the steps:
(1) the preparation of blank solution:
Weigh 1.0g cesium chloride, be placed in 100mL measuring bottle, be dissolved in water and be settled to scale, for subsequent use as ionization buffer, get 1mL ionization buffer and be placed in 10mL measuring bottle, then be diluted to scale with ultrapure water, shake up, to obtain final product;
(2) the preparation of need testing solution:
Get DANHONG ZHUSHEYE 0.2mL and be placed in counteracting tank, add 4mL red fuming nitric acid (RFNA), the 10min time-to-climb of in microwave dissolver, clear up 30min in 200 DEG C, after cooling, take out observation, solution clear, without insolubles, digestion solution is heated near dry, adds ultrapure water dilution, be transferred to 50mL measuring bottle, wash counteracting tank with dilution, and be progressively transferred to measuring bottle, add dilution to scale, shake up, as sodium/potassium ion test sample stock solution; Get test sample stock solution 3.125mL to put in 50mL measuring bottle, add 5mL ionization buffer, ultrapure water is diluted to scale, shakes up, as sodion need testing solution; Get test sample stock solution 2mL to put in 10mL measuring bottle, add 1mL ionization buffer, ultrapure water is diluted to scale, shakes up, as potassium ion need testing solution;
(3) the preparation of sodium/potassium ion reference substance solution:
Precision measures sodium/potassium ion standard solution, is placed in measuring bottle, is diluted with water to scale, shake up, and obtaining concentration is 10 μ gmL
-1ion standard working solution; Get sodium/potassium ion standard working solution, add ionization buffer respectively, ultrapure water is diluted to measuring bottle scale, shakes up, as sodium/potassium ion reference substance solution;
(4) assay:
Atomic absorption spectrophotometry is adopted to detect the absorbance of reference substance solution, drawing standard curve; And detect the absorbance of need testing solution, calculate content.
6. the detection method of sodium/potassium content in the DANHONG ZHUSHEYE as described in as arbitrary in claim 1-5, it is characterized in that, described mensuration sodium ions content, use the condition of work of Atomic Absorption Spectrometer as follows: to measure wavelength: 589.0nm, sodium spectrum bandwidth: 2nm, lamp current: 2mA, negative high voltage (-V): 300, gas flow 1.1min
-1, burner height: 5.0nm; Adopt air-acetylene flame.
7. the detection method of sodium/potassium content in the DANHONG ZHUSHEYE as described in as arbitrary in claim 1-5, it is characterized in that, described mensuration potassium content, use the condition of work of Atomic Absorption Spectrometer as follows: to measure wavelength: 766.9nm, potassium spectral bandwidth: 2nm, lamp current: 2mA, negative high voltage (-V): 300, gas flow: 1.7min
-1, burner height: 5.0nm; Adopt air-acetylene flame.
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| CN107219176A (en) * | 2017-05-18 | 2017-09-29 | 东莞市中鼎检测技术有限公司 | Using the method for sodium content in subsensitive line aas determination food |
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| CN110618188A (en) * | 2019-09-20 | 2019-12-27 | 成都第一制药有限公司 | Method for detecting content of cations in motherwort injection |
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| CN113406026A (en) * | 2021-06-15 | 2021-09-17 | 河北冀衡赛瑞化工有限公司 | Method for measuring content of potassium oxide in fertilizer by using flame atomic absorption spectrometer |
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