CN109358137A - A method of terramycin content in measurement oxytetracycline calcium pre-mixing agent - Google Patents
A method of terramycin content in measurement oxytetracycline calcium pre-mixing agent Download PDFInfo
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- CN109358137A CN109358137A CN201811595050.3A CN201811595050A CN109358137A CN 109358137 A CN109358137 A CN 109358137A CN 201811595050 A CN201811595050 A CN 201811595050A CN 109358137 A CN109358137 A CN 109358137A
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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
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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
- G01N2030/042—Standards
- G01N2030/047—Standards external
Abstract
The present invention relates to a kind of methods of terramycin content in measurement oxytetracycline calcium pre-mixing agent, belong to analysis and testing technology field, this method is high performance liquid chromatography, and chromatographic condition is as follows: C18 chromatographic column；Column temperature: 30-40 DEG C；Detection wavelength: 270-380nm；Mobile phase: the mixed liquor that phosphoric acid solution and the N,N-dimethylformamide that concentration is 2mmol/L are formed after 780-820:180-220 is mixed by volume；Pump discharge: 0.8-1.2mL/min；Sampling volume: 20 μ L；Runing time: 15-25min.Terramycin Standard Stock solutions, terramycin working standard solution and terramycin test solution are prepared, carries out efficient liquid phase chromatographic analysis according still further to above-mentioned chromatographic condition, carries out the calculating of terramycin content using peak area external standard method.This method favorable reproducibility, accuracy height, wider linear test scope and excellent durability, detect speed and precision are substantially better than bioassay.
Description
Technical field
The invention belongs to analysis and testing technology fields, and in particular to terramycin content in a kind of measurement oxytetracycline calcium pre-mixing agent
Method.
Background technique
Oxytetracycline calcium pre-mixing agent is the whole beer and appropriate calcium carbonate of terramycin production bacterium as a kind of feed addictive
Manufactured calcium salt of terramycin, active constituent are terramycin.
In veterinary drug national standard, oxytetracycline calcium premix agent content is measured using Microbiological methods.Practice have shown that
Have several drawbacks using microbiology polymorphism content: 1) influence factor of method is more, has to the accuracy of content measuring biggish
It influences；2) method is cumbersome, takes a long time, and causes working efficiency low；3) testing cost is higher.These defects restrict industrialization
Oxytetracycline calcium pre-mixing agent production process and quality control are produced, causes production efficiency low, quality control is unstable.
In view of the foregoing, oxytetracycline calcium pre-mixing agent content detection can accurately and reliably be detected and improve by being badly in need of one kind
Detection efficiency and the method for reducing inspection cost.
Summary of the invention
In view of this, the purpose of the present invention is to provide a kind of sides of terramycin content in measurement oxytetracycline calcium pre-mixing agent
Method.
In order to achieve the above objectives, the invention provides the following technical scheme:
1, a kind of method for measuring terramycin content in oxytetracycline calcium pre-mixing agent, the method is high performance liquid chromatography,
Chromatographic condition are as follows:
Chromatographic column: C18；
Column temperature: 30-40 DEG C；
Detection wavelength: 270-380nm；
Mobile phase: the phosphoric acid solution and N,N-dimethylformamide 780-820:180- by volume that concentration is 2mmol/L
The mixed liquor formed after 220 mixing；
Pump discharge: 0.8-1.2mL/min；
Sampling volume: 20 μ L；
Runing time: 15-25min.
Preferably, the high performance liquid chromatography specifically comprises the following steps:
(1) prepare terramycin Standard Stock solutions: take terramycin standard items with concentration be 0.05mol/L HCl solution it is dilute
The terramycin Standard Stock solutions that compound concentration is 500 μ g/mL are released, it is spare；
(2) terramycin working standard solution is prepared: using terramycin Standard Stock solutions in step (1) as mother liquor concentration
The terramycin working standard solution that compound concentration is 100 μ g/mL is diluted for the HCl solution of 0.05mol/L, crosses 0.22 μm of filter
Film, it is spare；
(3) prepare terramycin test solution: take oxytetracycline calcium pre-mixing agent sample with concentration be 0.05mol/L HCl it is molten
Terramycin test solution is prepared in liquid dilution, crosses 0.22 μm of filter membrane, spare；The reason of terramycin in the terramycin test solution
It is 0.4-500 μ g/mL by concentration；
(4) it is tested using high performance liquid chromatograph: the terramycin working standard solution of same volume and terramycin being taken to supply
Test sample solution, injects high performance liquid chromatograph, and chromatographic condition described in accordance with the claim 1 carries out efficient liquid phase chromatographic analysis；
Content calculating is carried out using peak area external standard method, calculation formula is as follows:
In formula:
AFor: for the peak area of terramycin in terramycin test solution map；
AWork: for the peak area of terramycin standard items in terramycin working standard solution map；
mMark: for the quality of terramycin standard items in terramycin Standard Stock solutions；
mFor: for the quality of oxytetracycline calcium pre-mixing agent sample in terramycin test solution；
N%: for the mass percent of terramycin standard items in terramycin Standard Stock solutions.
Preferably, in step (3), the theoretical concentration of terramycin is 100 μ g/mL in the terramycin test solution.
The beneficial effects of the present invention are: the present invention provides terramycin contents in a kind of measurement oxytetracycline calcium pre-mixing agent
Method, this method are high efficiency liquid phase chromatographic analysis method, have not only greatly improved detection speed and precision, while also ing save inspection
Cost is tested, specifically:
(1) the fast and accurately measurement of terramycin content, the achievable data acquisition of the every 25min of longest, phase are realized
Than Microbiological methods, detection efficiency is improved hundreds times, while greatly reducing the inspection cost of sample.
(2) reproducible, continuous 6 sample introductions measure the same sample, measure the RSD of terramycin content up to 0.05%,
And injection by bioassay is used, the RSD of general 6 measurements is 3% or so.
(3) reproducibility is good, different instruments is used by different inspectors, in not same date, respectively to same a collection of oxytetracycline calcium
Pre-mixing agent sample detection detects 6 times, and up to 0.44%, the RSD of far smaller than custom requirements is not more than testing result totality RSD
5% requirement.
(4) accuracy is high, is tested by the rate of recovery it is found that the rate of recovery of terramycin up to 99.2-100.4%, meets often
Advise desired rate of recovery 95-105% range.
(5) wider linear test scope, terramycin (are equivalent to oxytetracycline calcium in the concentration range of 0.5-250 μ g/mL
Contain terramycin 0.1-50wt% in pre-mixing agent) there is good linear dependence, related coefficient is up to 0.9996.
(6) quantitative limit and detection limit, for the quantitative limit of terramycin up to 0.07wt%, detection is limited to 0.018wt%, completely full
The requirement of foot measurement sample.
(7) durability is good: in a certain range, changing column temperature, changes flow, change mobile phase ratio, changes chromatographic column
Batch carries out system suitability test, and RSD is respectively less than 1.0%, and column effect, separating degree, tailing factor meets the requirements.
Detailed description of the invention
In order to keep the purpose of the present invention, technical scheme and beneficial effects clearer, the present invention provides following attached drawing and carries out
Illustrate:
Fig. 1 is efficient liquid phase typical case's chromatogram of oxytetracycline calcium pre-mixing agent sample in embodiment 2；
Fig. 2 is the high-efficient liquid phase chromatogram of terramycin working standard solution in the present invention；
Fig. 3 is linear regression of the terramycin working standard solution within the scope of concentration 0.5-250 μ g/mL in embodiment 5
Analyze curve.
Specific embodiment
Below by a preferred embodiment of the present invention will be described in detail.
Reagent used in test process and drug: purified water (HPLC grades), hydrochloric acid (excellent pure grade), phosphoric acid (top grade
It is pure), N,N-dimethylformamide (chromatographically pure)；
It prepares 2.0mol/L hydrochloric acid solution: measuring concentrated hydrochloric acid 84mL with purified water and be diluted to 500mL；
It prepares 0.05mol/L hydrochloric acid solution: measuring 2mol/L hydrochloric acid 25mL with purified water and be diluted to 1000mL；
It prepares 2mol/L phosphoric acid solution: measuring phosphatase 11 35mL with purified water and be diluted to 1000mL；
It prepares 2mmol/L phosphoric acid solution: taking 2mol/L phosphoric acid solution 0.8mL, purified water is added and is diluted to 800mL.
Prepare terramycin Standard Stock solutions: accurately weighed terramycin standard items 25.0mg is transferred to the volumetric flask of 50mL
In, it is dissolved with 0.05mol/L HCl, and be diluted to scale, is saved backup at 2-8 DEG C in refrigerator after shaking up；
It prepares terramycin working standard solution: taking above-mentioned terramycin Standard Stock solutions 5mL in 25mL volumetric flask, use
0.05mol/L HCl is diluted to scale, is configured to terramycin working standard solution, crosses 0.22 μm of filter membrane, spare；
Terramycin test solution is prepared as follows: taking specification is the oxytetracycline calcium pre-mixing agent sample of 20wt%, essence
Close weighed 50mg, is transferred in the volumetric flask of 100mL, infiltrates sample with 0.05mol/L hydrochloric acid, then uses 0.05mol/L again
HCl is diluted to scale, in stirring 30min on magnetic stirring apparatus, crosses 0.22 μm of filter membrane, spare.
Detecting instrument and condition:
Shimadzu LC-20A series and LC-2010CHT type high performance liquid chromatograph；
Chromatographic condition:
Chromatographic column: C18,5 μm of packing material size, the aperture of chromatographic column and length are 4.6 × 100mm/150mm；
Column temperature: 35 DEG C；
Detection wavelength: 280nm；
Mobile phase: phosphoric acid solution and the N,N-dimethylformamide that concentration is 2mmol/L are after 800:200 is mixed by volume
The mixed liquor of formation；
Pump discharge: 1.00mL/min；
Sampling volume: 20 μ L；
Runing time: 18min.
Embodiment 1
System suitability test
The terramycin working standard solution for taking above-mentioned preparation is carried out continuously 5 analyses, carries out the system suitability of method
Test is tested the repeatability (RSD) of chromatographic parameter peak area, column effect (N), tailing factor (T) separating degree (R), is surveyed
Test result is counted in the following table 1.
1 system suitability parameter testing result of table statistics
| Parallel analysis | Peak area | Column imitates (N) | Tailing factor (T) | Separating degree (R) |
| 1 | 3475859 | 3138 | 1.4 | 2.8 |
| 2 | 3479630 | 3161 | 1.4 | 2.8 |
| 3 | 3461801 | 3170 | 1.3 | 2.7 |
| 4 | 3451919 | 3165 | 1.3 | 2.7 |
| 5 | 3446269 | 3180 | 1.3 | 2.7 |
| Average value | 3463095 | 3163 | 1.3 | 2.7 |
| s | 14543 | / | / | / |
| RSD% | 0.42 | / | / | / |
As shown in Table 1, system suitability parameter testing result meets custom requirements.
Embodiment 2
Sample repeatability test
The terramycin working standard solution for taking above-mentioned preparation, according to above-mentioned terramycin test solution preparation method with same
A collection of oxytetracycline calcium pre-mixing agent is 6 parts of terramycin test solutions of sample preparation, carries out 6 measurements, carries out as follows
Test: by the terramycin working standard solution and terramycin test solution of same volume, it is efficient to inject Shimadzu LC-20A type
Liquid chromatograph is analyzed according to above-mentioned chromatographic condition, is recorded the retention time and peak area of 6 measurement terramycin, is passed through
Formula:The calculating of terramycin content is carried out, is as a result seen
Table 2.Wherein efficient liquid phase typical case's chromatogram of this batch of oxytetracycline calcium pre-mixing agent sample, as shown in Figure 1；Terramycin working standard
Solution high-efficient liquid phase chromatogram, as shown in Figure 2.
2 sample repeatability test data statistical form of table
| Terramycin test solution | Retention time | Terramycin peak area | Terramycin content (%) |
| 1 | 5.921 | 4039390 | 20.72 |
| 2 | 5.930 | 4038295 | 20.72 |
| 3 | 5.936 | 4038116 | 20.72 |
| 4 | 5.944 | 4038035 | 20.71 |
| 5 | 5.947 | 4040905 | 20.73 |
| 6 | 5.962 | 4043512 | 20.74 |
| Average value | 5.940 | 4039709 | 20.72 |
| Standard deviation | 0.014 | 2160 | 0.010 |
| RSD6 | 0.24% | 0.053% | 0.048% |
As shown in Table 2, the same terramycin test solution is measured continuous 6 times, the RSD of terramycin peak retention time is
0.24%；Peak area RSD is 0.053%；The RSD for measuring content is 0.048%, meets the requirement that RSD is not more than 2.0%.
Embodiment 3
The test of sample reproducibility
Reproducibility is also known as method precision, by different inspectors in not same date using different instruments to same
Product are detected to determine.
The terramycin working standard solution for taking above-mentioned preparation, according to above-mentioned terramycin test solution preparation method with same
A collection of oxytetracycline calcium pre-mixing agent is 6 parts of terramycin test solutions of sample preparation (respectively by two inspectors on the different dates
It prepares respectively, and respectively on Shimadzu LC-20 series type (instrument 1) and LC-2010CHT type high performance liquid chromatograph (instrument 2)
Injection), 6 measurements are carried out, are tested as follows: the terramycin working standard solution and soil of same volume is mould
Plain test solution injects in instrument, carries out analysis measurement according to above-mentioned chromatographic condition, pass through formula: The calculating of terramycin content is carried out, and records measurement knot
Fruit statisticallys analyze the RSD of measurement result, is shown in Table 3.
3 sample reproducibility (method precision) test data of table statistical analysis
As shown in Table 3, different instruments are used by different inspectors, in not same date, it is pre- to same a collection of oxytetracycline calcium respectively
Mixture sample detection 6 times, testing result totality RSD is 0.44%, meets the requirement that conventional RSD is not more than 3%.
Embodiment 4
Sample accuracy test
Accuracy is the degree of closeness between measured value and true value, and the accuracy of representation method is usually carried out with the rate of recovery.
The oxytetracycline calcium pre-mixing agent sample (terramycin content is 20.57wt%) of specification known to one is selected, it is dilute with 0.05mol/L HCl
It releases, prepares the other oxytetracycline calcium pre-mixing agent sample solution of 3 concentration levels respectively, each rank is prepared 3 parts, totally 9 parts, carried out 9 times
Analysis measurement, carries out according to above-mentioned chromatographic condition every time, then passes through formula: The calculating of terramycin content is carried out, and records measurement result, and then calculates measurement terramycin every time
The rate of recovery (measured value/theoretical value), as a result see the table below 4.
4 accuracy test data of table statistics
As shown in Table 4, the rate of recovery of terramycin is 99.2-100.4%, meets the rate of recovery in the requirement of 95-105%.
Embodiment 5
Linear and its range test
Prepare a series of terramycin working standard solution (minimum of the interval comprising tested sample of various concentration
With peak), injection measurement is carried out respectively, and linear regression analysis is carried out to determination data.
Above-mentioned terramycin Standard Stock solutions are diluted, it is (relatively dense centered on terramycin working standard solution
100%) degree, carries out the diminution and expansion of concentration, prepares the other terramycin working standard solution of 11 concentration levels, final dilute
Releasing concentration see the table below 5, and range is from 0.5-250 μ g/mL.By the working standard solution of 11 concentration according to above-mentioned chromatographic condition
Analysis test is carried out, respectively recording responses peak area, each concentration and response peak area are subjected to linear regression analysis.Regression analysis
Curve is as shown in figure 3, linear fit obtains regression equation are as follows: linearly dependent coefficient is calculated in y=0.00003x+1.2699
R2It is 0.9996.Measurement results are shown in Table 5.
5 terramycin of table is linear and range test data
As shown in Table 5, terramycin (is equivalent in oxytetracycline calcium pre-mixing agent containing gold in the concentration range of 0.5-250 μ g/mL
Mycin 0.1-50wt%) there is good linear dependence, related coefficient 0.9996.
Embodiment 6
Detection limit and quantitative limit measure
Corresponding detectable concentration is used as quantitative limit when being usually 10 using signal-to-noise ratio (S/N), when with signal-to-noise ratio (S/N) being 3 pair
The detectable concentration answered is as detection limit.In embodiment 5 in the terramycin range of linearity on the basis of minimum concentration, to terramycin work
Continuing dilution metering as standard solution, test result shows that the signal-to-noise ratio (S/N) when concentration is 0.35 μ g/mL is 10,
I.e. using this concentration as quantitative limit (being equivalent to 0.07wt%)；Signal-to-noise ratio (S/N) when concentration is 0.09 μ g/mL is 3, i.e., this
Concentration is as detection limit (being equivalent to 0.018wt%).
Embodiment 7
Durability test
By carrying out small change to chromatographic condition, system suitability test is carried out, again to examine or check the durable of method
Property, can see, which reach expected, receives standard (RSD≤2% of swarming area).This test is the change point by following condition
Not carry out method durability examination, test result is shown in Table 6.
1) change column temperature, tested under conditions of 35 DEG C ± 5 DEG C respectively.
2) change flow velocity, tested under the flow velocity of 1.00 ± 0.1mL/min respectively.
3) change mobile phase ratio, tested under conditions of mobile phase composition transfer ± 10%, receiving mark should be met
Standard, specific experimental condition are carried out by the following two kinds situation:
Mobile phase 1:2mmol/L phosphoric acid solution/n,N-Dimethylformamide, volume ratio 780:220
Mobile phase 2:2mmol/L phosphoric acid solution/n,N-Dimethylformamide, volume ratio 820:180
4) change chromatographic column, tested using the chromatographic column (length is respectively 100mm and 150mm) of different batches.
6 method serviceability test of table statistics
As shown in Table 6, system suitability measurement is carried out by the change of chromatographic condition as above again, measurement result meets
Receive standard (peak area and the RSD of retention time are no more than 2%), this shows that this method is relatively stable, durable.
Finally, it is stated that preferred embodiment above is only used to illustrate the technical scheme of the present invention and not to limit it, although logical
It crosses above preferred embodiment the present invention is described in detail, however, those skilled in the art should understand that, can be
Various changes are made to it in form and in details, without departing from claims of the present invention limited range.
Claims (3)
1. a kind of method of terramycin content in measurement oxytetracycline calcium pre-mixing agent, which is characterized in that the method is efficient liquid phase
Chromatography, chromatographic condition are as follows:
Chromatographic column: C18；
Column temperature: 30-40 DEG C；
Detection wavelength: 270-380nm；
Mobile phase: 780-820:180-220 is mixed by volume for the phosphoric acid solution and N,N-dimethylformamide that concentration is 2mmol/L
The mixed liquor formed after conjunction；
Pump discharge: 0.8-1.2mL/min；
Sampling volume: 20 μ L；
Runing time: 15-25min.
2. the method for terramycin content in a kind of measurement oxytetracycline calcium pre-mixing agent according to claim 1, which is characterized in that
The high performance liquid chromatography specifically comprises the following steps:
(1) terramycin Standard Stock solutions are prepared: taking the HCl solution that terramycin standard items are 0.05mol/L with concentration to dilute and matches
Concentration processed is the terramycin Standard Stock solutions of 500 μ g/mL, spare；
(2) it prepares terramycin working standard solution: being using terramycin Standard Stock solutions in step (1) as mother liquor with concentration
The terramycin working standard solution that the HCl solution dilution compound concentration of 0.05mol/L is 100 μ g/mL, crosses 0.22 μm of filter membrane,
It is spare；
(3) prepare terramycin test solution: take oxytetracycline calcium pre-mixing agent sample with concentration be 0.05mol/L HCl solution it is dilute
It releases and prepares terramycin test solution, cross 0.22 μm of filter membrane, it is spare；The theory of terramycin is dense in the terramycin test solution
Degree is 0.4-500 μ g/mL；
(4) it is tested using high performance liquid chromatograph: taking the terramycin working standard solution and terramycin test sample of same volume
Solution, injects high performance liquid chromatograph, and chromatographic condition described in accordance with the claim 1 carries out efficient liquid phase chromatographic analysis；
Content calculating is carried out using peak area external standard method, calculation formula is as follows:
In formula:
AFor: for the peak area of terramycin in terramycin test solution map；
AWork: for the peak area of terramycin standard items in terramycin working standard solution map；
mMark: for the quality of terramycin standard items in terramycin Standard Stock solutions；
mFor: for the quality of oxytetracycline calcium pre-mixing agent sample in terramycin test solution；
N%: for the mass percent of terramycin standard items in terramycin Standard Stock solutions.
3. the method for terramycin content in a kind of measurement oxytetracycline calcium pre-mixing agent according to claim 2, which is characterized in that
In step (3), the theoretical concentration of terramycin is 100 μ g/mL in the terramycin test solution.
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Application publication date: 20190219 |