CN109060973B - Method for detecting ethylenediamine in lipoic acid injection - Google Patents
Method for detecting ethylenediamine in lipoic acid injection Download PDFInfo
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- CN109060973B CN109060973B CN201810701011.0A CN201810701011A CN109060973B CN 109060973 B CN109060973 B CN 109060973B CN 201810701011 A CN201810701011 A CN 201810701011A CN 109060973 B CN109060973 B CN 109060973B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
Abstract
The invention specifically relates to a method for detecting ethylenediamine in a lipoic acid injection, which comprises the following steps: 1) preparing ethylene diamine into a reference solution; 2) preparing a test solution from the zinc sulfate injection; 3) respectively detecting the reference solution and the test solution by adopting an ion chromatography, and calculating the content of the ethylenediamine; wherein the chromatographic conditions of the ion chromatography comprise the following contents: a chromatographic column: the stationary phase is cation exchange resin or chemical bonding ion exchanger; mobile phase: the mobile phase A is methanesulfonic acid, and the mobile phase B is methanol or acetonitrile; the volume ratio of the mobile phase A to the mobile phase B is 90-98: 10-2. The ion chromatography is adopted to detect the ethylenediamine, so that the ethylenediamine can be effectively detected, and the detection result is accurate, the base line is smooth, the peak shape is symmetrical, the stability is high, the repeatability is good, and the sensitivity is high.
Description
Technical Field
The invention relates to the field of detection methods, in particular to a method for detecting ethylenediamine.
Background
The ethylene diamine is colorless or yellowish oily or water sample liquid, has an ammonia-like smell, has a boiling point of 116-117.2 ℃, is strongly alkaline and corrosive, and is mainly used for solvents and analytical reagents.
The ethylenediamine is a pH value regulator and a cosolvent which are commonly used in the medicine, and the food and drug supervision and administration requires a special method to control the content of the ethylenediamine in the medicine approval and tightens the limit. In the prior art, the gas chromatography is adopted to measure the ethylenediamine, but the ethylene diamine has high corrosivity to a sample feeding system, and is easy to tail and branch in a chromatographic column, so that the sample feeding precision is poor, and the limit requirement of the marked quantity of +/-5% cannot be met.
Disclosure of Invention
At present, no relevant report for determining the ethylenediamine in the lipoic acid injection by adopting an ion chromatography is found in the prior art. The applicant researches and discovers that the chromatogram obtained by measuring the ethylenediamine by adopting the cation chromatography has symmetrical peak pattern and smooth base line, and the method also has the characteristics of high sensitivity, good stability and good reproducibility.
The invention provides a method for detecting ethylenediamine in a lipoic acid injection, which comprises the following steps:
1) preparing ethylene diamine into a reference solution;
2) preparing a test solution from the zinc sulfate injection;
3) respectively detecting the reference solution and the test solution by adopting an ion chromatography, and calculating the content of the ethylenediamine; wherein the chromatographic conditions of the ion chromatography comprise the following contents:
a chromatographic column: the stationary phase is cation exchange resin or chemical bonding ion exchanger;
mobile phase: the mobile phase A is organic acid, and the mobile phase B is methanol or acetonitrile; the volume ratio of the mobile phase A to the mobile phase B is 90-98: 10-2.
The calculation of the content of the ethylenediamine can adopt conventional methods such as an external standard method, an internal standard method, an area normalization method and the like. When the internal standard method is used, the internal standard substance is selected to be a substance which does not interfere with the absorption peak of ethylenediamine, and can be obtained by the prior art and some routine experiments. In one embodiment of the invention, an external standard method is adopted for calculation, so that the method is simple and convenient.
In one embodiment of the invention, the concentration of the organic acid is 5-50 mmol/L; including but not limited to 8mmol/L, 10mmol/L, 18mmol/L, 22mmol/L, 27mmol/L, 32mmol/L, 36mmol/L, 41mmol/L, 47mmol/L, etc. In one embodiment of the present invention, the concentration is preferably 15 mmol/L. The organic acid is preferably methanesulfonic acid.
In an embodiment of the present invention, the mobile phase B is acetonitrile. Compared with methanol, the method has better elution capability, can generate peaks more quickly on the basis of good detection effect, and simultaneously greatly reduces the detection cost.
In one embodiment of the invention, the volume ratio of the mobile phase A to the mobile phase B is 90-92: 10-8; preferably, the volume ratio is 90:10 or 92: 8.
In one embodiment of the present invention, the solvent for preparing the control solution or the test solution is one or more selected from a group consisting of methanesulfonic acid solution, methanol, acetonitrile, and water. The invention preferably uses water as the solvent, has good compatibility with instruments, improves the detection precision and sensitivity and improves the detection accuracy.
In one embodiment of the invention, the chromatographic column is RFIC IonPac, CS 17; further, the length of the chromatographic column is 250-500mm, and the inner diameter is 3-5 mm; a preferred column has a length of 250mm and an internal diameter of 4 mm.
In one embodiment of the invention, the flow rate of the mobile phase is 0.6-1 ml/min; preferably 0.8 ml/min.
In one embodiment of the invention, the temperature of the chromatographic column is 25-40 ℃; preferably 30 deg.c.
In one embodiment of the invention, the sample volume of the method is 5-50 μ l; further experiments found that when selected from 10. mu.l, the asymmetry is low and the chromatographic symmetry is good.
Wherein the conductance detector is selected from conductance detectors with suppressors. The detection method adopts a conventional method, and can also carry out some simple transformations according to actual conditions, and the transformations are routine operations in the field.
The invention has the beneficial effects that:
the method adopts the ion chromatography to detect the ethylenediamine, uses the acidic mobile phase for elution, can effectively detect the ethylenediamine, and has the advantages of accurate detection result, smooth base line, symmetrical peak shape, high stability, good repeatability, high separation degree, low detection limit and high sensitivity.
Secondly, the recovery rate of the ethylenediamine by adopting the method of the invention reaches 97.57-100.71%, and the RSD% is 0.98%.
Drawings
FIG. 1 is a linear graph of ethylenediamine;
FIG. 2 limits of quantitation of ethylenediamine;
FIG. 3 is a graph of a blank dissolution chromatogram peak of the IC method;
FIG. 4 chromatographic peaks for an ethylenediamine control solution;
FIG. 5 is a chromatogram peak diagram of a test solution.
Detailed Description
The raw materials and equipment used in the embodiment of the invention are known products, and can be obtained by purchasing commercially available products, and the details are as follows:
1. the instrument comprises the following steps:
ion chromatography: DIONEX ICS1100 ion chromatograph-DionexAS-DV injector, detector: conductance detector, workstation: chromeleon 6.80SR9a Build 2680 (163077).
Ion Chromatography (IC) column: RFICTM 
CS17(4 × 250mm), Ion Chromatography (IC) guard column: RFICTM 
CG17(4 × 250mm), suppressor: dionex CERS 5004 mm.
Gas chromatograph: agilent 7890B gas chromatograph, detector: hydrogen Flame Ionization Detector (FID)
A GC chromatographic column: SE-30 capillary column (30m 0.32mm 0.5 μm), DB-WAX capillary column (30m 0.53mm 1.0 μm), DB-1 capillary column (30m 0.53mm 3.0 μm)
Balance: mettlettoloedoxa 205DU one-ten-thousandth of a balance; sartorius sartorius CPA255D one-tenth-ten-thousandth balance
A liquid transferring gun: sartorius BioHit pipette (10-100. mu.l; 20-200. mu.l; 100-1000. mu.l; 1000-5000. mu.l)
2. Reagents and reagents:
water is ultrapure water (sartoriumpro), methanesulfonic acid (chromatographically pure, CNW), acetonitrile (chromatographically pure, Fisher);
ethylenediamine (analytically pure, Chengdu Kelong chemical reagent factory, lot number 2017011101, purity ≥ 99.0%)
3. Sample preparation:
lipoic acid injection (batch No. 170701, 170702, 170703, Kyokute Teper pharmaceutical Co., Ltd., specification: 12ml:300mg)
| Composition (I) | Dosage of | Function of |
| Lipoic acid | 300mg | Active ingredient |
| Ethylene diamine | About 80mg | pH regulator |
| Water for injection | 12ml | Solvent(s) |
| Medicinal charcoal | 4.8mg | Adsorbent and process for producing the same |
| Nitrogen gas | Proper amount of | Inert gas |
Lipoic acid injection (batch No. 62402, Germany Steadde pharmaceutical factory, size 12ml:300mg)
Lipoic acid bulk drug (batch 20170601, Dudoute Teddy Co., Ltd.)
The traditional method for detecting the ethylenediamine in the lipoic acid injection comprises the following steps:
the traditional detection method comprises the following steps: ethylene diamine was measured by gas chromatography (appendix VE of the second part of the Chinese pharmacopoeia, 2010). A detector: a hydrogen flame ionization detector at a temperature of 320 ℃; sample inlet temperature: 320 ℃; the split ratio was 50: 1. A chromatographic column: the fixative was a polydimethylsiloxane (SE-30,30m 0.32mm 0.5um) capillary column. The column temperature was started at 100 ℃ for 3min, and increased to 280 ℃ at a rate of 50 ℃ per minute for 15 min. Preparation of control solutions: taking a proper amount of ethylenediamine, precisely weighing, adding dimethyl sulfoxide: water (1:1) was dissolved and diluted to make a control solution containing about 3.4mg per 1 ml. Test solution: precisely measuring 5ml of the product, placing into a 10ml measuring flask, adding appropriate amount of dimethyl sulfoxide to dissolve and dilute to scale, and shaking uniformly. The determination method comprises injecting 1ul of each of the reference solution and the sample solution into a gas chromatograph, and recording chromatogram; calculating according to the peak area by an external standard method to obtain the product. Detecting to obtain the content of the ethylenediamine of 6.003mg/ml-7.337 mg/ml.
The applicant adopts gas chromatography and external standard method calculation according to the original reported standard, and respectively adopts SE-30 capillary column (30m 0.32mm 0.5 μm), DB-WAX capillary column (30m 0.53mm 1.0 μm) and DB-1 capillary column (30m 0.53mm 3.0 μm) to find that: because the concentration of the ethylenediamine is higher, the alkalinity is relatively higher, the corrosion of a sample feeding system is larger, the tailing and peak bifurcation are easy to occur in a chromatographic column, the sample feeding precision is poorer, and the limit requirement of +/-5 percent cannot be met. Wherein the peak shape and tailing phenomenon of the DB-1 capillary column are superior to those of other capillary chromatographic columns, so that the DB-1 capillary column is selected for continuous research and study.
Considering that the precision is reduced probably due to the sampling by an external standard method, selecting an internal standard method experiment, correcting and eliminating the deviation caused by the sampling, adopting weakly alkaline organic pyridine as an internal standard substance, adjusting the temperature rise condition of a program, slightly improving the tailing phenomenon of ethylenediamine, and ensuring good separation degree of ethylenediamine and pyridine, but in the experiment, the chromatographic column effect has an obvious decline trend after continuous experiments for about one week, and in the continuous sampling process, data from one needle to two needles are suddenly abnormal occasionally, the relative deviation is large, the same sample is subjected to parallel sampling twice, and the relative deviation of the experimental result is 6.1%; the sample introduction precision (n is 6) RSD of the reference substance reaches 3.2 percent, which indicates that the ethylene diamine has strong corrosion and damage effects on a chromatographic column by adopting a gas phase method for determination, and results are easy to be abnormal after long-time experiments.
Applicants further tested the ethylenediamine study using ion chromatography, examples are as follows:
example one
And (3) detecting the content of ethylenediamine in the lipoic acid injection:
a chromatographic column: RFIC IonPac CG17, 4mm x 50mm, CS17, 4mm x 250 mm;
mobile phase: 15mmol/L methanesulfonic acid is used as a mobile phase A, acetonitrile is used as a mobile phase B, and the volume ratio is 9: 1;
a detector: the detector is a conductivity detector with a suppressor CERS500, 4 mm;
feeding amount: 10 mu l of the mixture;
column temperature: 30 ℃;
flow rate: 0.8 ml/min;
a detection step:
precisely measuring 1ml of the product, placing into a 100ml measuring flask, adding water to dissolve, diluting to scale, and shaking to obtain a test solution; and taking an ethylenediamine reference substance, precisely weighing, adding water to dissolve, and quantitatively diluting a 66.7 mu g/ml solution to serve as a reference substance solution. Precisely measuring 10 μ l of each of the test solution and the reference solution, injecting into an ion chromatograph, recording chromatogram, and calculating according to external standard method by peak area. The results are as follows:
the lipoic acid injection (170701, 170702, 170703) and the reference preparation lipoic acid injection (batch No. 62402, German Standd) were used for determination according to the proposed examination method. The results are shown in Table 1, run 170703 with duplicate experimental data.
TABLE 1 examination of ethylenediamine in lipoic acid injection
The measured results all meet the limitation requirement of +/-5% of the marked quantity.
Example two
The applicants fully consider the chemical nature of ethylenediamine and make measurements using a conductivity detector. Because the ethylenediamine substance characteristic still obviously trails on the chromatographic column, the mobile phase and the sample injection volume are further screened by taking the asymmetry as an index, and the screening conditions are shown in table 2.
TABLE 2IC chromatographic Condition screening
When the applicant examines the addition amount of acetonitrile, when the volume percentage is more than 10%, the retention time of the ethylenediamine is less than 5min, which is not favorable for detection, and the inhibition signal is enhanced with the increase of the addition amount of the acetonitrile, so that the ratio of the methyl sulfonic acid: the volume ratio of acetonitrile is 90: 10.
Research shows that by using the methanesulfonic acid as a mobile phase, the retention time of the ethylenediamine is advanced along with the increase of the concentration of the methanesulfonic acid, and the retention time gradually tends to 5min when the concentration of the methanesulfonic acid exceeds 15mmol/L, so that the preferable concentration of the methanesulfonic acid is 15mmol/L, the retention time is short, the detection speed is high, and the solvent is saved.
Studies have also found that the asymmetry of ethylenediamine increases with increasing sample volume.
In conclusion, the chromatographic condition 5 is selected as the optimal chromatographic condition, the retention time of the ethylenediamine is about 5.3min, and the asymmetry degree is 1.31.
To further illustrate the beneficial effects of the detection method of the present invention, the present invention provides the following test examples.
The following detection conditions were used:
a chromatographic column: RFIC IonPac CG17, 4mm x 50mm, CS17, 4mm x 250 mm;
mobile phase: 15mmol/L methanesulfonic acid is used as a mobile phase A, acetonitrile is used as a mobile phase B, and the volume ratio is 9: 1;
a detector: the detector is a conductivity detector with a suppressor CERS500, 4 mm;
feeding amount: 10 mu l of the mixture;
column temperature: 30 ℃;
flow rate: 0.8ml/min
Preparing a solution:
(1) 0.3343g and 0.3348g of ethylenediamine are precisely weighed out from the reference substance stock solution, placed in a 50ml measuring flask, dissolved in water and diluted to scale, and shaken up for later use, wherein the concentrations are 6.686mg/ml and 6.696mg/ml respectively.
(2) The reference substance solution is precisely measured to obtain 1ml of reference substance stock solution, the reference substance stock solution is placed in a 100ml measuring flask, water is added to dilute the reference substance stock solution to a scale mark, and the reference substance stock solution is shaken up to have concentrations of 66.86 mu g/ml and 66.96 mu g/ml respectively.
(3) Precisely measuring 1ml of sample (enterprise: Doctorbai special pharmaceutical Co., Ltd., lot: 170703) in a 100ml measuring flask, adding water to dissolve and dilute to scale, and shaking up to obtain the final product.
1. System suitability test
Ion chromatography using a cation exchange column (
CG17(4mm x 50mm), CS17(4mm x 250 mm)); the detector is a conductivity detector (with suppressor CERS500, 4 mm); precisely measuring blank solvent, ethylenediamine reference solution and sample solution, sampling 10 μ l each, and recording chromatogram as shown in FIGS. 4-5. The theoretical plate numbers and degrees of separation are shown in Table 3 below.
TABLE 3 theoretical plate number of ethylenediamine and degree of separation
The results show that: the blank solvent does not interfere with the determination of the component to be detected; no interference of other impurity peaks exists in the reference substance solution and the sample solution; the number of theoretical plates of the peak to be measured is more than 3000, and the peak shape is good.
2. Linear experiment
Taking a reference substance stock solution for dilution to obtain linear standard solutions with different concentrations, wherein the specific dilution steps are as follows: precisely measuring control stock solution (6.696mg/ml)0.5ml, 0.8ml, 1.0ml, 1.2ml, 1.5ml and 2.0ml respectively, placing into 100ml measuring flask, adding water to dissolve and dilute to scale, and shaking.
And sampling the solutions, and recording a chromatogram. Taking the concentration as an abscissa and the peak area of the component to be measured as an ordinate, drawing a standard curve of each component, wherein a linear graph is shown in figure 1:
TABLE 4 Linear relationship of ethylenediamine
And (3) test results: the linear equation of the ethylenediamine is that Y is 0.0181X +0.4584, the correlation coefficient R is 0.9988, and the result shows that the linear relation of the ethylenediamine is good in the range of 33.48 mu g/ml to 133.92 mu g/ml.
3. Limit of quantification
Precisely measuring a proper amount of reference solution (66.96 mu g/ml), diluting by 1000 times step by step, injecting into an ion chromatograph, and recording chromatogram. The sample amount when the signal-to-noise ratio (S/N) is about 10 is the limit of quantitation, and through conversion, the limit of quantitation of ethylenediamine is 0.75 μ g/ml, and the chromatogram is shown in figure 2.
4. Accuracy test
Precisely weighing about 1.25g of lipoic acid raw material medicine (batch number 20170601), placing the lipoic acid raw material medicine into a 50ml measuring flask, adding a small amount of acetonitrile to dissolve the lipoic acid raw material medicine, adding water to dilute the lipoic acid raw material medicine until the lipoic acid raw material medicine is uniformly shaken in scales, precisely weighing 1ml of the lipoic acid raw material medicine into a 100ml measuring flask, precisely adding 0.8ml, 1ml and 1.2ml of reference substance stock solution (the concentration is about 6.6mg/ml) into the reference substance stock solution respectively, dissolving the three parts respectively according to a preparation method of a prepared sample, using the dissolved reference substance stock solution as test solutions of 80%, 100% and 120% of recovery rate tests, and detecting the results according to prepared chromatographic conditions, wherein the results are shown in a table 5.
TABLE 5 ethylenediamine recovery
The results show that: the recovery rate of the ethylenediamine is 97.57-100.71%, the RSD% is 0.98%, and the result shows that the method has high accuracy and can accurately detect the ethylenediamine in the sample.
5. In-day precision test
A reference solution (with a concentration of about 66.7. mu.g/ml) was measured and injected into a liquid chromatograph, and the samples were continuously injected 6 times, respectively, and the chromatogram was recorded, and the precision was examined, and the results are shown in Table 6.
TABLE 6 results of precision test
The test result shows that the retention time of the ethylenediamine chromatographic peak and the RSD of the peak area are both less than 1.0 percent, which indicates that the product has good daily precision.
6. Stability of solution
The control solutions were measured and injected into a liquid chromatograph at 0 hour, 4 hours, 6 hours, 8 hours, and 24 hours, respectively, and the results of the chromatogram and the solution stability were examined are shown in table 7.
TABLE 7 stability of the solutions
The test results showed that the control solution was stable over 24 hours.
7. Repeatability test
1ml and 6 parts of sample (batch No. 170703) are precisely measured, a test solution is prepared according to a proposed method, each part is horizontally moved by two needles according to the method for measurement, a chromatogram is recorded, and the content of ethylenediamine is inspected, and the results are shown in Table 8.
TABLE 8 results of the repeatability tests
The test results show that the contents of ethylenediamine in 6 parts of samples have no significant difference, the RSD values are all less than 1.0%, and the repeatability is good.
8. Day time precision test
The product was taken and measured by ion chromatography for three days, respectively, and the precision during the day was examined, and the results are shown in Table 9.
TABLE 9 results of day precision test
The test result shows that the RSD percent of the content determination result of the ethylenediamine in different time (three days) is less than 2.0 percent, and the precision in the daytime is good.
9. Durability
Taking lipoic acid injection (170701) and a reference preparation, lipoic acid injection (batch No. 62402, Germany Standd), respectively adjusting the flow rate to 1.0ml/min according to durability 1, adjusting the flow rate to 0.6ml/min according to durability 2, adjusting the column temperature to 35 ℃ according to durability 3, adjusting the detection cell temperature to 40 ℃, and adjusting the mobile phase to be 15mmol/L methanesulfonic acid according to durability 4: acetonitrile (92:8), the chromatographic conditions were adjusted, and ethylenediamine was measured by the method, and the results are shown in Table 10.
TABLE 10 durability test results
Test results show that the RSD% of the ethylene diamine content is less than 1.5% when the chromatographic conditions are changed to a certain extent, and the method has good durability.
10. Limit determination
According to the requirement of national CDE center supplement opinion, the limit requirement is increased to 6.33-7.00 mg of ethylenediamine contained in each 1 ml.
In conclusion, the method for detecting the content of the ethylenediamine in the lipoic acid injection provided by the invention is simple and convenient to operate, easy to control, low in detection cost, good in linear relation, specificity, precision, stability, sensitivity and repeatability, high in sample recovery rate accuracy, good in method repeatability, accurate and reliable in detection result, and capable of providing an effective method for accurately detecting the content of the ethylenediamine and ensuring the product quality of the zinc sulfate injection.
The above description is only an embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be made by those skilled in the art without inventive work within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope defined by the claims.
Claims (10)
1. A method for detecting ethylenediamine in a lipoic acid injection is characterized by comprising the following steps:
1) preparing ethylene diamine into a reference solution;
2) preparing a sample solution from a lipoic acid injection;
3) respectively detecting the reference solution and the test solution by adopting an ion chromatography, and calculating the content of the ethylenediamine;
wherein the chromatographic conditions of the ion chromatography comprise the following contents:
a chromatographic column: cation exchange resin is used as a stationary phase; mobile phase: the mobile phase A is 15mmol/L methanesulfonic acid, and the mobile phase B is acetonitrile; the volume ratio of the mobile phase A to the mobile phase B is 90-92: 10-8;
the flow rate of the mobile phase is 0.6-1 ml/min;
the column temperature of the chromatographic column is 25-40 ℃.
2. The method for detecting ethylenediamine in lipoic acid injection according to claim 1, wherein the method comprises the following steps: the volume ratio is 90:10 or 92: 8.
3. The method for detecting ethylenediamine in lipoic acid injection according to claim 1 or 2, characterized in that: the solvent for preparing the reference substance solution or the test solution is one or more selected from a methanesulfonic acid solution, methanol, acetonitrile and water.
4. The method for detecting ethylenediamine in lipoic acid injection according to claim 3, wherein the method comprises the following steps: the solvent for preparing the reference solution or the test solution is water.
5. The method for detecting ethylenediamine in lipoic acid injection according to claim 1, wherein the method comprises the following steps: the chromatographic column is RFIC IonPac, CS 17.
6. The method for detecting ethylenediamine in lipoic acid injection according to claim 1, wherein the method comprises the following steps: the length of the chromatographic column is 250-500mm, and the inner diameter is 3-5 mm.
7. The method for detecting ethylenediamine in lipoic acid injection according to claim 1, wherein the method comprises the following steps: the flow rate of the mobile phase was 0.8 ml/min.
8. The method for detecting ethylenediamine in lipoic acid injection according to claim 1, wherein the method comprises the following steps: the column temperature of the column was 30 ℃.
9. The method for detecting ethylenediamine in lipoic acid injection according to claim 1, wherein the method comprises the following steps: the sample amount of the method is 5-50 μ l.
10. The method for detecting ethylenediamine in lipoic acid injection as recited in claim 9, wherein the method comprises the following steps: the amount of sample was 10. mu.l.
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| CN111007194B (en) * | 2019-12-29 | 2022-07-19 | 无锡殷达尼龙有限公司 | Method for quantifying sodium ion content in nylon monomer by using ion chromatography |
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