CN105044248B - The quantitative detecting method of natrium adetate and sodium pyrosulfite in a kind of ginseng and astragalus injection for strengthening body - Google Patents
The quantitative detecting method of natrium adetate and sodium pyrosulfite in a kind of ginseng and astragalus injection for strengthening body Download PDFInfo
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Abstract
The present invention establishes the quantitative detecting method of natrium adetate and sodium pyrosulfite in a kind of quantitative analysis ginseng and astragalus injection for strengthening body, includes the following steps：Prepare natrium adetate and sodium pyrosulfite reference substance solution；Prepare ginseng and astragalus injection for strengthening body test solution；Using the above-mentioned reference substance solution of ion chromatography quantitative analysis and test solution；According to EDTA in reference substance and sample ions chromatogram2‑And SO3 2‑、SO4 2‑Ion chromatography peak peak area, according to S element conservation principles in solution, respectively according to natrium adetate and EDTA2‑, sodium pyrosulfite and SO3 2‑、SO4 2‑Molar ratio and molecular weight conversion sample in the content of natrium adetate and sodium pyrosulfite.
Description
Technical field
It is specifically a kind of to pass through the present invention relates to a kind of method for ginseng and astragalus injection for strengthening body safety control and application
Establish the chromatography of ions additives natrium adetate and sodium pyrosulfite that are added in ginseng and astragalus injection for strengthening body are detected and
The method of application belongs to Pharmaceutical Analysis technology and safety control field.
Background technology
Ginseng and astragalus injection for strengthening body is that national Chinese medicine protects kind, protects kind number：ZYB2072004073, be by Radix Astragali and
The big infusion of Chinese medicine, for qi deficiency lung cancer, the auxiliary treatment of gastric cancer, can improve the immune work(of body made of Radix Codonopsis is extracted
Can, and Cardial or cerebral vascular diseases can be treated, have effects that strengthen the body resistance to consolidate the constitution, is QI invigorating qi-restoratives, promoting blood circulation and removing blood stasis.
Ginseng and astragalus injection for strengthening body complicated component, the data according to disclosed in ZL 201210436493.4, in finger-print only
Characteristic peak just has as many as 18；According to ZL 201310008395.5, the ingredient hairiness stamen that ginseng and astragalus injection for strengthening body identifies is different
Flavones -7-O- β-D-Glucose glycosides, different dimpling sword-like leave Sha alcohol -7,2 '-two-O- glucosides, biochanin -7- glucose
Glycosides, 9,10- dimethoxy red sandalwood alkane -3-O- xylose glucoses glycosides, Astragaloside IV, 5 hydroxymethyl furfural etc. are many known and not
The ingredient known brings great difficulty to the quality control of ginseng and astragalus injection for strengthening body.In order to keep the controllability of parenteral solution quality
And stability, the method for the high accuracy analysis such as infrared spectrum, nuclear magnetic resonance, high performance liquid chromatography are all applied to monitoring ginseng in succession
S peaks (Calycosin-7-O-BETA-D-glucoside) and the larger water soluble ingredient of polarity in astragalus injection for strengthening body, Astragaloside content, its it is negatively correlated into
Point, saponin component etc..Even if numerous advanced analyzing detecting methods be used for ginseng and astragalus injection for strengthening body quality control, but in order to
It checks erroneous ideas at the outset, increases clinical application safety, the research of ginseng and astragalus injection for strengthening body quality control is never interrupted.
While miscellaneous ingredient brings great difficulty to the quality control of ginseng and astragalus injection for strengthening body, also one is caused to production
Fixed puzzlement.When preparing intravenously administrable infusion, generally using rustless steel container and pipeline, under heating state, parenteral solution and gold
After belonging to the contact of the long periods such as container, pipeline, filter, the component of parenteral solution can be combined with substances such as metal ions, and generation is coloured
Metal composite, solution colour is caused to deepen, main ingredient reacts with metal ion in order to prevent, reduce solution changes color, this
Be added to suitable metal chelating agent natrium adetate and antioxidant sodium pyrosulfite in product, additive amount be about 0.2g/L and
0.5g/L。
Some researches show that natrium adetate can cause the reduction of calcium with calcium binding into soluble complex compound, quiet now
Blood calcium can be caused to decline using natrium adetate in arteries and veins preparation, if excessive addition can cause blood calcium too low, nausea, headache, urgent urination,
The adverse reactions such as blood coagulability reduction；There is document report：If human body largely takes in natrium adetate, natrium adetate can be with
Calcium in blood and bone forms water soluble chelate compound, is excreted, causes low blood calcium or bone calcium loss, leads to twitch even
It is dead.In addition, sodium pyrosulfite is in the solution with SO3 2-And SO4 2-Form exist, storage it is long, can also release SO2。SO2
There is apparent stimulation to skin, mucous membrane, conjunctiva, bronchitis symptom can be caused；Its hyposulfite can also cause allergy.
The target user of ginseng and astragalus injection for strengthening body is qi deficiency lung cancer, patients with gastric cancer, and physical function is weak, immunity degradation, it is easier to be produced
The adverse reactions such as raw allergy, headache, it is therefore desirable to stringenter control natrium adetate and sodium pyrosulfite usage amount.Although
Metal chelating agent natrium adetate and antioxidant sodium pyrosulfite are added in ginseng and astragalus injection for strengthening body, but is directed to additional
Disclosed method of quality control is not yet established in agent.The uncertain factors such as personnel's emotional instability in process of production may be led
The deviation of inventory is caused, brings quality and security risk.In order to ensure the safety of clinical application, need to natrium adetate and coke
Sodium sulfite establishes method of quality control.
Invention content
The present invention provides additives natrium adetate in a kind of ion chromatography quantitative analysis control ginseng and astragalus injection for strengthening body
With the method for pyrosulfurous acid sodium content, it is specifically related to natrium adetate and sodium pyrosulfite in a kind of ginseng and astragalus injection for strengthening body
Quantitative detecting method.
It is a further object of the present invention to provide the applications of above-mentioned quantitative detecting method.
In some documents, in drug injection liquid during micro ion sulfate by ion chromatography, parenteral solution is directly injected into
It is analyzed in ion chromatographic column.The complicated component of ginseng and astragalus injection for strengthening body, as stated in the Background Art, wherein containing amino acid,
All multicomponents such as carbohydrate (mainly monosaccharide and oligosaccharides), organic acid, sodium chloride, up to 18 kinds of a variety of different chemical substances with
On, and the content of 2 kinds of additives of natrium adetate and sodium pyrosulfite is low, through overtesting, find by parenteral solution be directly injected into from
In sub- chromatographic column, the chlorion peak area as a result shown on chromatogram is excessively high, accounts for more than the 95% of whole Component peak areas；Simultaneously
Chromatographic column column effect declines quickly, and retention time fluctuation is big, and the spectrogram caused can not be understood, and can not detect edetic acid(EDTA) at all
Disodium and sodium pyrosulfite.
In order to solve problem above, inventor gropes by various, finds after sample is diluted, can be substantially
Degree reduces the peak area of chlorion, but chromatographic column column effect still has decline to the ginseng and astragalus injection for strengthening body after diluting in the detection
Soon, the problem of retention time fluctuation is big.
In the documents and materials having disclosed, ZL 201310756866.0 injects body resistance-strengthening ginseng-astragalus with magnetic nuclear resonance method
When liquid carries out quality control, ginseng and astragalus injection for strengthening body have passed through frozen dried；ZL201310008395.5, ginseng and astragalus injection for strengthening body
It is handled through 0.45 μm of miillpore filter filter；ZL 201210436493.4 is handled using the filtration of 0.22um miillpore filters；ZL
It in 200710136382.0, is filtered by macroreticular resin, the processing steps such as extraction.Inventor is by the processing means in open source literature
It is applied in the present invention, can not all solve column effect and decline the technical issues of fast.
By the ginseng and astragalus injection for strengthening body that arduous experiment, our pleasantly surprised discoveries were diluted using the processing of C18 columns, chlorine
Ion peak areas interference is eliminated, and chromatographic column column effect is not decreased obviously, and the fluctuation of retention time is controllable, can be with accurate quantification
Detect natrium adetate and sodium pyrosulfite.
The quantitative detecting method of natrium adetate and sodium pyrosulfite in a kind of ginseng and astragalus injection for strengthening body of the present invention, including with
Lower step：
(1) with the EDTA of natrium adetate and sodium pyrosulfite in sulfate by ion chromatography ginseng and astragalus injection for strengthening body2-、
SO3 2-、SO4 2-Ion concentration；
(2) calculating of natrium adetate and sodium pyrosulfite：
The calculating of natrium adetate：The EDTA according to step (1)2-Concentration, according to natrium adetate and EDTA2-1
: 1 molar ratio is converted into the concentration of natrium adetate in solution；
The calculating of sodium pyrosulfite：1. by areas of peak normalization method, using drawing Na2S2O5During reference substance standard curve
SO in the Working Control solution of various concentration3 2-And SO4 2-Peak area, calculate Na2S2O5SO in solution3 2-And SO4 2-Ratio；
2. according to Na2S2O5In reference substance solution, SO3 2-And SO4 2-Ratio and S element conservations, according to Na2S2O5Respectively with SO3 2-With
SO4 2-Molar ratio, converted by the molecular weight of three, draw SO respectively3 2-And SO4 2-Standard curve；3. according to sample solution
Middle SO3 2-And SO4 2-Peak area, substitute into SO respectively3 2-And SO4 2-Standard curve, calculate SO3 2-And SO4 2-Concentration, further according to point
Son amount is converted into SO3 2-And SO4 2-Molar concentration；4. according to S element conservations in solution, according to SO3 2-And SO4 2-It is mole dense
Degree calculates Na2S2O5Molar concentration, and then according to molecular weight calculate sample in Na2S2O5Concentration.
Ginseng and astragalus injection for strengthening body described in step (1) first passes through the small column purifications of C18, and then eluent dilutes 50-400 times
Afterwards, then pass through ion chromatographic column.
Ginseng and astragalus injection for strengthening body described in step (1) first passes through the small column purifications of C18, and then eluent dilutes 100-200 times
Afterwards, then pass through ion chromatographic column.
Ginseng and astragalus injection for strengthening body described in step (1) first passes through the small column purifications of C18, after then eluent dilutes 200 times, then
Pass through ion chromatographic column.
The preparation of reference substance solution is further included in the step (1), takes natrium adetate, sodium pyrosulfite reference substance respectively
In right amount, it is accurately weighed, add water that every 1mL solution containing natrium adetate, 1 μ g of sodium pyrosulfite respectively is made.
The chromatographic chromatographic condition of step (1) intermediate ion is：Chromatographic column is IonPac AS11-HC (4 × 250mm),
Potassium hydroxide solution of the eluent concentration for 0~30min 15mmol/L, electric conductivity detector, flow velocity 1mL/min, sample size are
25μL。
The control method of natrium adetate and sodium pyrosulfite provided by the invention can be applied to ginseng and astragalus injection for strengthening body
The measure of middle additives can effectively evaluate the safety of ginseng and astragalus injection for strengthening body.
Compared with prior art, the invention has the advantages that：
In ginseng and astragalus injection for strengthening body quality standard and its relevant research data, not yet to its additives natrium adetate and
Sodium pyrosulfite is controlled, and excessive natrium adetate and sodium pyrosulfite has human body damage, and the special kind is quiet
Arteries and veins injection, the larger , Qi of risk need to be evaluated and controlled to the safety of additives.Therefore the method for the present invention establishes ion chromatography
The technical standard of natrium adetate and sodium pyrosulfite in method detection ginseng and astragalus injection for strengthening body, passes through quantitative analysis EDTA2-With
SO3 2-、5O4 2-, the dosages of drug additives can be fast and effeciently monitored, in addition to the operation rule in the source strict control personnel that feed intake
Outside model, a kind of approach of monitoring drug additives dosage after feed intake, double control, safety of ensuring drug quality are additionally provided.Together
When the present invention can with real-time quantitative measure EDTA2-、SO3 2-And SO4 2-Amount, for accurately calculating ginseng and astragalus injection for strengthening body product
The surplus of natrium adetate and sodium pyrosulfite in storage, so as to accurate evaluation coke natrium adetate and sodium sulfite
Whether inventory is reasonable, and the inventory of final accurate adjustment natrium adetate and sodium pyrosulfite reaches to greatest extent with most
Science inventory, most effective quality control as a result, optimization drug additives use, ensure drug safety.It is in addition, of the invention
In by simultaneously measure SO3 2-And SO4 2-The method for calculating pyrosulfurous acid sodium content in sample has certain advanced, its stability
It is preferable with reproducibility, the detection of other preparations can be applied to.
Description of the drawings
Fig. 1 is natrium adetate reference substance chromatography of ions figure；
Fig. 2 is sodium pyrosulfite reference substance chromatography of ions figure；
Fig. 3 is the chromatography of ions figure of ginseng and astragalus injection for strengthening body sample；
Fig. 4 is the chromatography of ions figure of pure water；
Fig. 5 is natrium adetate canonical plotting；
Fig. 6 is inferior sulfate radical canonical plotting；
Fig. 7 is sulfate radical canonical plotting；
Fig. 8 is the chromatography of ions figure of ginseng and astragalus injection for strengthening body difference extension rate；
Fig. 9 is the chromatography of ions figure that ion chromatographic column is Biobasic；
Figure 10 is the chromatography of ions figure that ion chromatographic column is AS11-HC；
Figure 11 is the chromatography of ions figure that ion chromatographic column eluent concentration is 15mMol/L；
Figure 12 is the chromatography of ions figure that ion chromatographic column eluent concentration is 13mMol/L；
Figure 13 is the chromatography of ions figure that ion chromatographic column eluent concentration is 11.5mMol/L；
Figure 14 is the chromatography of ions figure that ion chromatographic column eluent concentration is 10mMol/L；
Figure 15 is the chromatography of ions figure of sample pre-treatments and sample injection time difference.
Specific embodiment
The technical solution further illustrated the present invention below by way of specific embodiment.
Embodiment 1
1 instrument and reagent
1.1 instrument：Ion chromatograph：DIONEX ICS-2000 (Dai An companies)；Chromatographic column：IonPac AS11-HC(4
× 250mm) (Dai An companies)；Guard column：IonPac AH11-HC (4 × 50mm) (Dai An companies)；Detector：Electric conductivity detector
(Dai An companies)；Elute flow container：EGCII KOH(090581489019).Millipore pure water meters.
1.2 reagent：Natrium adetate reference substance (lot number：20100311, Hangzhou Li Ren pharmaceutcal corporation, Ltds)；Pyrosulfurous acid
Sodium reference substance (lot number：20100301, Hunan Er-kang Pharmaceutical Co., Ltd.).Sep-Pak Cartridges Vac C18 3cc are small
Column (Waters).Ginseng and astragalus injection for strengthening body is provided by Livzon Group Limin Pharmaceutical Factory.Agents useful for same acetonitrile, formic acid are equal in experiment
For chromatographically pure, water is ultra-pure water.
2 methods and result
The preparation of 2.1 test solutions：Precision measures ginseng and astragalus injection for strengthening body 1mL, by the small column purifications of C18, spend from
Sub- water elution, constant volume 10mL measuring bottles, then the accurate 2.5mL that measures in 50mL measuring bottles, constant volume to get.
The preparation of 2.2 reference substance solutions：Respectively accurately weighed natrium adetate, sodium pyrosulfite reference substance 0.01140g,
0.01168g is dissolved in water in 100mL measuring bottles and is diluted to scale, compareed respectively as natrium adetate, sodium pyrosulfite
Product storing solution.
2.3 chromatographic condition：Chromatographic column is IonPac AS11-HC (4 × 250mm), and eluent concentration is 0~30min
The potassium hydroxide solution of 15mmol/L, electric conductivity detector, flow velocity 1mL/min, sample size are 25 μ L.
2.4 linear relationship
2.4.1 the linear relationship of natrium adetate
Natrium adetate reference substance storing solution is diluted respectively, prepares a series of solution of standard curve：4.56、
3.42nd, 2.28,1.14,0.57 μ g/mL, sample introduction is analyzed under above-mentioned chromatographic condition, records reference substance peak area.With reference substance peak
Area is ordinate, and a concentration of abscissa draws reference substance standard curve：Y=0.039x-0.0087, r=0.9990, as a result table
Bright natrium adetate linear relationship in the concentration range of 0.57~4.56 μ g/mL is good.
2.4.2 the linear relationship of sodium pyrosulfite
Due to Na2S2O5In water with SO3 2-And SO4 2-Form exist, using measuring SO respectively3 2-And SO4 2-Method,
It is converted into Na2S2O5Content (S conservations).
Na2S2O5+H2O=2NaHSO3(sodium pyrosulfite water suction)
2NaHSO3+O2=2NaHSO4(sodium hydrogensulfite oxidation)
It can also be reacted by the niter cake of oxidation generation with the sodium pyrosulfite or sodium hydrogensulfite not absorbed water：
2NaHSO4+Na2S2O5=2Na2SO4+2SO2+H2O
NaHSO3+NaHSO4=Na2SO4+SO2+H2O
Sodium pyrosulfite storing solution is diluted respectively, prepares a series of solution of standard curve：4.672、3.504、
2.336th, 1.168,0.584 μ g/mL, 25 μ L of sample introduction, record reference substance peak area respectively.First, by areas of peak normalization method,
Calculate Na2S2O5In solution, SO3 2-And SO4 2-Ratio (being shown in Table 1)：
1 SO of table3 2-And SO4 2-In Na2S2O5Distribution in solution
According to Na2S2O5In solution, SO3 2-And SO4 2-Ratio and S element conservations, draw SO respectively3 2-And SO4 2-Mark
Directrix curve：
①SO3 2-Standard curve：Y=0.112x-0.0089, r=0.9985 (table 2).
2 SO of table3 2-Standard curve
| Working curve (μ g/ml) | Peak area |
| 2.805 | 0.313 |
| 2.334 | 0.246 |
| 1.497 | 0.153 |
| 0.775 | 0.078 |
| 0.381 | 0.038 |
②SO4 2-Standard curve：Y=0.0942x-0.0031, r=0.9992 (table 3).
3 SO of table4 2-Standard curve
| Working curve (μ g/ml) | Peak area |
| 1.355 | 0.126 |
| 0.740 | 0.065 |
| 0.564 | 0.048 |
| 0.250 | 0.021 |
| 0.132 | 0.011 |
2.5 precision test：Take ginseng and astragalus injection for strengthening body (lot number：0910499), by the preparation method system of test solution
Standby, continuous sample introduction 6 times measures the content of natrium adetate and sodium pyrosulfite, the results showed that precision is good (being shown in Table 4).
4 precision test of table
2.6 repetitive test：It takes with a collection of ginseng and astragalus injection for strengthening body (lot number：1001015), totally 6 parts, sample introduction, is surveyed respectively
Determine the content of natrium adetate and sodium pyrosulfite, the results showed that this law repeatability is good (being shown in Table 5).
5 repetitive test of table
2.7 recovery test：It takes with a collection of ginseng and astragalus injection for strengthening body (lot number：1001015) 1mL, totally 6 parts, according to repetition
Property and the linear theoretical content for calculating natrium adetate and sodium pyrosulfite, add in the natrium adetate and sodium pyrosulfite of equivalent
Reference substance dilutes one times, calculates the rate of recovery according to the actually measured value of natrium adetate and sodium pyrosulfite, the results showed that according to ground
For the rate of recovery of acid disodium and sodium pyrosulfite between 90%~110%, the method accuracy is good (being shown in Table 6, table 7).
The preparation of recycling reference substance solution：Respectively precision weigh natrium adetate and sodium pyrosulfite 0.02163g,
0.05145g is configured to the mixed reference substance solution of natrium adetate and sodium pyrosulfite, then accurate absorption in 100mL measuring bottles
1mL is added in test sample.
The rate of recovery of 6 natrium adetate of table is investigated
The rate of recovery of 7 sodium pyrosulfite of table is investigated
2.8 stability
2.8.1 sample stability is investigated
Take ginseng and astragalus injection for strengthening body (lot number：1001015), respectively at 0,2,4,8,12 hour sample introduction, edetic acid(EDTA) two is recorded
The peak area of sodium and sodium pyrosulfite, the results showed that sample is good (being shown in Table 8) in 12 hours internal stabilities.
8 study on the stability of table
2.8.2 sodium pyrosulfite study on the stability
Due to Na2S2O5In aqueous solution with SO3 2-And SO4 2-Form exist, and SO3 2Further reaction it can generate SO2,
It is necessary to its stability is investigated.Precision weighs Na2S2O50.01189g is configured to a concentration of 1.189 μ g/mL solution,
Respectively at 0,2,4,6,8,10,12 hour sample introduction, SO is recorded3 2-And SO4 2-Peak area.The result shows that sodium pyrosulfite is water-soluble
Two ions in liquid are good (being shown in Table 9) in 12 hours internal stabilities.
9 Na of table2S2O5Study on the stability
Natrium adetate and pyrosulfurous acid sodium determination application example in 2.9 ginseng and astragalus injection for strengthening body
Natrium adetate in ginseng and astragalus injection for strengthening body and sodium pyrosulfite are carried out using the chromatography of ions of above-mentioned foundation
It measures, can quickly and accurately analyze the content of additives, the safety of ginseng and astragalus injection for strengthening body be controlled, while right
The dosage of enterprises adjustment additives has certain directive significance.The measurement result of part batch is shown in Table 10, the results show that sample
Natrium adetate content is basically identical with inventory (0.2g to 1000ml) between 0.163~0.198mg/mL in product；Jiao Ya
The content of sodium sulphate is basically identical with inventory (0.5g to 1000ml) through converting between 0.445~0.537mg/mL.As a result
Show that additional agent content in the ginseng and astragalus injection for strengthening body detected using this method and its inventory are basically identical, available for this
The evaluation of kind safety.
Natrium adetate and sodium pyrosulfite measurement result in 10 sample segment of table
Therefore, using natrium adetate and sodium pyrosulfite in ion-chromatographic determination ginseng and astragalus injection for strengthening body, Ke Yiyou
Effect ground controls the safety of the product, ensures the safety and stability of the kind clinical application.
The screening of 2 ginseng and astragalus injection for strengthening body extension rate of embodiment
The preparation of test solution：
Test solution 1：10 times of dilution
Precision measures ginseng and astragalus injection for strengthening body 1mL, and by the small column purifications of C18, de-, constant volume 10mL amounts are washed with deionized water
Bottle, constant volume to get.
Test solution 2：20 times of dilution
Precision measures ginseng and astragalus injection for strengthening body 1mL, and by the small column purifications of C18, de-, constant volume 10mL amounts are washed with deionized water
Bottle, then the accurate 2.5mL that measures is in 5mL measuring bottles, constant volume to get.
Test solution 3：50 times of dilution
Precision measures ginseng and astragalus injection for strengthening body 1mL, and by the small column purifications of C18, de-, constant volume 10mL amounts are washed with deionized water
Bottle, then the accurate 10mL that measures is in 50mL measuring bottles, constant volume to get.
Test solution 4：100 times of dilution
Precision measures ginseng and astragalus injection for strengthening body 1mL, and by the small column purifications of C18, de-, constant volume 10mL amounts are washed with deionized water
Bottle, then the accurate 5mL that measures is in 50mL measuring bottles, constant volume to get.
Test solution 5：200 times of dilution
Precision measures ginseng and astragalus injection for strengthening body 1mL, and by the small column purifications of C18, de-, constant volume 10mL amounts are washed with deionized water
Bottle, then the accurate 2.5mL that measures is in 50mL measuring bottles, constant volume to get.
Test solution 6：400 times of dilution
Precision measures ginseng and astragalus injection for strengthening body 1mL, and by the small column purifications of C18, de-, constant volume 10mL amounts are washed with deionized water
Bottle, then the accurate 2.5mL that measures is in 100mL measuring bottles, constant volume to get.
Other experimental implementation schemes are with reference to described in embodiment 1, experimental result is shown in Fig. 8 and such as the following table 11：
Table 11
| Inferior sulfate radical area | Sulfate radical area | Inferior sulfate radical/sulfate radical | |
| Test solution 6 | 4.225 | 2.071 | 2.04 |
| Test solution 5 | 9.963 | 4.492 | 2.22 |
| Test solution 4 | 20.034 | 9.037 | 2.22 |
| Test solution 3 | 41.994 | 18.656 | 2.25 |
| Test solution 2 | 108.105 | 47.352 | 2.28 |
| Test solution 1 | 221.663 | 94.701 | 2.34 |
As seen from the figure, as extension rate increases, the response of chlorion is substantially reduced, and is effectively reduced to system
Pollution；Meanwhile considered according to instrument signal to noise ratio, inferior sulfate radical and sulfate radical ratio stability, the peak area of inferior sulfate radical
It is advisable in the peak area of 10 or so, sulfate radical in 5 or so, ratio 2.2 or so.Therefore 200 times of selection dilution.
3 chromatographic column of embodiment selects
Two kinds of ion chromatographic columns of AS11-HC and Biobasic are compared, experiment condition is with reference to described in embodiment 1, experiment knot
Fruit such as chromatogram 9 and 10.
AS11-HC figure baselines are steady, and separating degree is schemed compared with Biobasic.Therefore selection AS11-HC ion chromatographic columns.
Embodiment 4：The selection of ion chromatographic column eluent concentration
The potassium hydroxide that eluent concentration examines 15mMol/L, 13mMol/L, 11.5mMol/L, 10mMol/L respectively is molten
Liquid, other experiment conditions are carried out according to embodiment 1.
Leacheate various concentration chromatogram is shown in 11-14.
According to chromatogram, leacheate is 11.5mMol/L and is with leacheate during the potassium hydroxide solution of 10mMol/L
15mMol/L is compared with the potassium hydroxide solution of 13mMol/L, and the baseline before inferior sulfate radical appearance is more steady, 11.5mMol/
The potassium hydroxide solution of L and 10mMol/L is more suitable for leacheate.
The potassium hydroxide solution phase for being 10mMol/L with leacheate during the potassium hydroxide solution that leacheate is 11.5mMol/L
Than appearance time is shorter, and in order to shorten analysis time, the preferably potassium hydroxide solution of 11.5mMol/L is as leacheate.
Embodiment 5：Sample pre-treatments and sample injection time
Oxidizable since inferior sulfate radical is unstable, sample stability examination situation is shown, sample introduction after sample is placed 8 hours,
As a result there is more apparent variation, thus sample should be completed to measure in 6 hours after processing.Should anticipate cut-back tank when handling sample simultaneously
Clean situation, thinned water should use the ultra-pure water (or with preceding use proper method deoxidation treatment) prepared in 2 hours.
Table 12
Embodiment 6：The screening of ginseng and astragalus injection for strengthening body pre-treatment step
Direct-injection technique：As a result chlorion peak area is excessively high, accounts for more than the 95% of whole Component peak areas；Chromatographic column simultaneously
Column effect declines quickly, and retention time fluctuation is big.
Dilute sampling system (but C18 columns)：Extension rate is investigated, it is 200 to determine extension rate, and as a result chlorion is dry
It disturbs and greatly reduces, but chromatographic column column effect still declines significantly.
200 times are diluted after 0.45 μm of filtering with microporous membrane：The interference of chlorion greatly reduces, but chromatographic column column effect still declines
Significantly.
200 times of dilution after after 0.22um filtering with microporous membrane：Under the interference of chlorion greatly reduces, but chromatographic column column is imitated still
Drop is apparent.
200 times are diluted after AB-8 macroreticular resin filtration treatments：The interference of chlorion greatly reduces, and chromatographic column column effect declines
To improvement, but retention time still fluctuates, it is impossible to meet analysis demand.
200 times are diluted after the filtering of C18 columns：The interference of chlorion greatly reduces, and chromatographic column column effect declines and improved, and retains
Time fluctuation is smaller, can meet analysis demand.
To sum up, preferably C18 columns are as the means pre-processed.
Claims (3)
1. the quantitative detecting method of natrium adetate and sodium pyrosulfite in a kind of ginseng and astragalus injection for strengthening body, includes the following steps：
(1) with the EDTA of natrium adetate and sodium pyrosulfite in sulfate by ion chromatography ginseng and astragalus injection for strengthening body2-、SO3 2-、
SO4 2-Ion concentration；
(2) calculating of natrium adetate and sodium pyrosulfite：
The calculating of natrium adetate：The concentration of EDTA2- according to step (1), according to natrium adetate and EDTA2-1: 1
Molar ratio, be converted into the concentration of natrium adetate in solution；
The calculating of sodium pyrosulfite：1. by areas of peak normalization method, using drawing Na2S2O5It is different during reference substance standard curve
SO in the Working Control solution of concentration3 2-With the peak area of SO42-, Na is calculated2S2O5SO in solution3 2-And SO4 2-Ratio；2. root
According to Na2S2O5In reference substance solution, SO3 2-And SO4 2-Ratio and S element conservations, according to Na2S2O5Respectively with SO3 2-And SO4 2-
Molar ratio, converted by the molecular weight of three, draw SO respectively3 2-And SO4 2-Standard curve；3. according in sample solution
SO3 2-And SO4 2-Peak area, substitute into SO respectively3 2-And SO4 2-Standard curve, calculate SO3 2-And SO4 2-Concentration, further according to molecule
Amount is converted into SO3 2-And SO4 2-Molar concentration；4. according to S element conservations in solution, according to SO3 2-And SO4 2-Molar concentration,
Calculate Na2S2O5Molar concentration, and then according to molecular weight calculate sample in Na2S2O5Concentration；
Ginseng and astragalus injection for strengthening body described in step (1) first passes through the small column purifications of C18, after then eluent dilutes 100-200 times, then
Pass through ion chromatographic column；
Wherein, the chromatographic chromatographic condition of step (1) intermediate ion is：Chromatographic column is AS11-HC, and specification is 4 × 250mm,
Potassium hydroxide solution of the eluent concentration for 0~30min 11.5mMol/L, electric conductivity detector, flow velocity 1mL/min, sample size
For 25 μ L.
2. the quantitative detection side of natrium adetate and sodium pyrosulfite in a kind of ginseng and astragalus injection for strengthening body as described in claim 1
Method, ginseng and astragalus injection for strengthening body described in step (1) first pass through the small column purifications of C18, after then eluent dilutes 200 times, then pass through
Ion chromatographic column.
3. the quantitative detection side of natrium adetate and sodium pyrosulfite in a kind of ginseng and astragalus injection for strengthening body as described in claim 1
Method, it is characterised in that the preparation of reference substance solution is further included in the step (1), takes natrium adetate, sodium pyrosulfite respectively
Appropriate reference substance, it is accurately weighed, add water that every 1mL solution containing natrium adetate, 1 μ g of sodium pyrosulfite respectively is made.
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