CN110146599A - A kind of detection method of content of Gamithromycin - Google Patents
A kind of detection method of content of Gamithromycin Download PDFInfo
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- G01N30/02—Column chromatography
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Abstract
The invention discloses a kind of detection method of content of Gamithromycin, this method is high performance liquid chromatography, is filler with octadecylsilane chemically bonded silica；Using acetonitrile-water-liquor ammoniae fortis of volume ratio 60-75:25-40:0.1 as mobile phase, survey wavelength is 208nm-220nm；Flow velocity is 0.8ml/min-1.2ml/min；Column temperature is 30 DEG C -40 DEG C, and external standard method quantifies sample.Compared with prior art, the present invention uses conventional detection apparatus, and flow visualizing is stablized, and detection data is reliable；The method is easy, and specificity, reproducibility, precision, linear, accuracy is good, and Gamithromycin purity is good, is not interfered by impurity；Chromatographic peak does not prolong before relatively, does not trail, and peak shape symmetry is good.
Description
Technical field
The present invention relates to Pharmaceutical Analysis technical fields, and in particular to a kind of detection method of content of Gamithromycin.
Background technique
Gamithromycin is 7 α class antibiotic of second generation macrolides azepine, molecular formula C40H76N2O12, molecular weight is
777.04, chemical name is (2R, 3S, 4R, 5S, 8R, 10R, 11R, 12S, 13S, 14R) -13- [(2,6- dideoxy -3-C- first
Base -3-O- methyl-α-L- core-hexpyranosyl) oxygen] -2- ethyl -3,4,10- trihydroxy -3,5,8,10,12,14- hexamethyl -
7- propyl -11- [[tri- deoxidation -3- (dimethylamino)-β-D- wood of 3,4,6--hexpyranosyl] oxygen] -1- oxa- -7- azacyclo- ten
Five alkane -15- ketone.Structural formula are as follows:
As the Macrocyclolactone lactone kind medicines such as azithromycin, Tulathromycin, tylonolide, Gamithromycin is to respiratory system disease
The therapeutic effect of disease is excellent, and drug concentration is easily accumulated in lung tissue, maintains effective blood drug concentration up to 10 weeks or more, can be effective
Ox respiratory disease caused by Mannheimia haemolytica, pasteurella multocida, sleep Histophilus is treated and prevented, in beast
Doctor is clinically with a wide range of applications.
But by literature search it can be found that the quality standard of Gamithromycin, and it is uncharged in USP United States Pharmacopeia, EP
In the foreign pharmacopeias such as European Pharmacopoeia, JP Japanese Pharmacopoeia, IP pharmacopoeia of India, for the medicament contg quantitative detecting analysis method without
Method inquires unified statutory standard foundation.Wherein, give that " a kind of Gamithromycin contains in patent CN201310745236
Quantity measuring method ", flow visualizing is acetonitrile: 0.025mol/ml dipotassium hydrogen phosphate solution (pH8-8.5)=70:30, at this
Buffer salt component dosage is larger in flow visualizing, is influenced mobile phase precipitation problem easily occur by factors such as environment, and efficient liquid
The flow line of phase equipment (HPLC) is thinner, so influence detection data stability or cause instrument and equipment blocking etc. ask
Topic；It is given in patent CN201510027705 " a kind of detection method of content of Gamithromycin ", detector is required using steaming
Light Scattering Detector, relative to UV detector, the diode array detector etc. being most widely used, the detector is opposite
It is special, so that the use of this method is restricted.
Summary of the invention
The present invention is in view of the defects existing in the prior art or insufficient, provides a kind of detection method of content of Gamithromycin, with
It solves in the prior art, when detecting Gamithromycin using high performance liquid chromatography, existing flow visualizing and detection data are not
The problem of stablizing, or needing special detection device.
Technical scheme is as follows:
A kind of detection method of content of Gamithromycin, this method are high performance liquid chromatography, are included the following steps:
Chromatographic condition and system suitability: being filler with octadecylsilane chemically bonded silica；With volume ratio 60-
Acetonitrile-water-liquor ammoniae fortis of 75:25-40:0.1 is mobile phase, and survey wavelength is 208nm-220nm；Flow velocity is 0.8ml/min-
1.2ml/min；Column temperature is 30 DEG C -40 DEG C；Number of theoretical plate is calculated by Gamithromycin peak should be not less than 5000；
The preparation of test sample: taking Gamithromycin accurately weighed, is quantitatively diluted and is made in every lml containing 0.5- with acetonitrile solution
The solution of 1.5mg；
The preparation of reference substance: taking Gamithromycin reference substance, ibid the preparation method preparation of test sample；
Measuring method: it is accurate respectively to measure above-mentioned 10 μ l of solution, liquid chromatograph is injected, chromatogram is recorded；By external standard method with
Calculated by peak area to get.
It is preferred according to the present invention, above-mentioned Gamithromycin detection method of content, instrument selection high performance liquid chromatograph
2998 detector of Agilent DAD detector or Waters is that common detector detects in medicine enterprise.
It is preferred according to the present invention, above-mentioned Gamithromycin detection method of content, the preferred Polar-RP C18 chromatography of chromatographic column
Column, peak shape are preferable；The Polar-RP C18 chromatographic column of further preferred Ultimate brand.
Preferred according to the present invention, above-mentioned Gamithromycin detection method of content, mobile phase is the second of volume ratio 65:35:0.1
Nitrile-water-liquor ammoniae fortis.
It is preferred according to the present invention, above-mentioned Gamithromycin detection method of content, the preferred 210nm of Detection wavelength.
It is preferred according to the present invention, above-mentioned Gamithromycin detection method of content, the preferred 1.0ml/min of flow velocity.
It is preferred according to the present invention, above-mentioned Gamithromycin detection method of content, preferably 40 DEG C of column temperature.
It is preferred according to the present invention, above-mentioned Gamithromycin detection method of content, in the preparation of the test sample, dilution second
Nitrile aqueous solution preferred volume ratio be 60%-75%, further preferably 65%.
It is preferred according to the present invention, above-mentioned Gamithromycin detection method of content, in the preparation of the test sample, dilution second
After nitrile aqueous dissolution measuring samples, Gamithromycin sample concentration is 1.0mg/ml.
According to the present invention it is further preferred that a kind of detection method of content of Gamithromycin, this method are high-efficient liquid phase color
Spectrometry, specific steps include:
Chromatographic condition and system suitability: being filler with octadecylsilane chemically bonded silica；With volume ratio 65:
Acetonitrile-water-liquor ammoniae fortis of 35:0.1 is mobile phase；Detection wavelength is 210nm；Flow velocity is 1.0ml/min；Column temperature is 40 DEG C；
Number of theoretical plate is calculated by Gamithromycin peak should be not less than 5000；
The preparation of test solution: taking this product accurately weighed, is quantitatively diluted and is made with 65% acetonitrile solution of volume ratio
Solution in every lml containing about 0.5-1.5mg；
The preparation of reference substance solution: taking Gamithromycin reference substance, ibid the preparation method preparation of test sample；
Measuring method: it is accurate respectively to measure above-mentioned 10 μ l of solution, liquid chromatograph is injected, chromatogram is recorded；By external standard method with
Calculated by peak area to get.
Following experimental examples are only used for further illustrating but are not limited to the present invention.
Experimental example 1: the specificity test of Gamithromycin content detection
Chromatographic condition and system suitability: Ultimate Polar-RP, 5 μm, 4.6 × 250mm chromatographic column；With body
Acetonitrile-water-liquor ammoniae fortis of the product than 65:35:0.1 is mobile phase；Detection wavelength is 210nm；Flow velocity is 1.0ml/min；Column temperature
It is 40 DEG C.Number of theoretical plate is calculated by Gamithromycin peak should be not less than 5000.2998 detector of Waters.
The preparation of test solution: taking this product accurately weighed, is quantitatively diluted and is made with 65% acetonitrile solution of volume ratio
Solution in every lml containing about 1.5mg.
The preparation of reference substance solution: Gamithromycin reference substance is taken, is measured in the same method.
Measuring method: it is accurate respectively to measure above-mentioned 10 μ l of solution, liquid chromatograph is injected, in 200~400nm wave-length coverage
3D scanning is carried out, Gamithromycin sample map is compared with Gamithromycin reference substance map.As a result it see the table below 1.Map is shown in attached drawing 1
With attached drawing 2.
The specificity test result of 1 Gamithromycin assay of table
| Sample message | Purity angle | Purity threshold value |
| Reference substance | 0.329 | 0.482 |
| Test sample | 0.467 | 0.476 |
Conclusion: the above specificity experiments have shown that, Gamithromycin peak purity angle be less than purity threshold value, it was demonstrated that peak be it is pure, add
The measurement of rice mycin is undisturbed, illustrates that this method specificity is strong.
Experimental example 2: instrument precision and the method precision test of Gamithromycin content detection
Chromatographic condition and system suitability: Agilengt1260 high performance liquid chromatograph DAD detector, Ultimate
Polar-RP, 5 μm, 4.6 × 250mm chromatographic column；Using acetonitrile-water-liquor ammoniae fortis of volume ratio 65:35:0.1 as mobile phase；Inspection
Survey wavelength is 210nm；Flow velocity is 1.0ml/min；Column temperature is 40 DEG C.Number of theoretical plate should be not less than by the calculating of Gamithromycin peak
5000。
The preparation of test solution: taking this product accurately weighed, quantitatively diluted with acetonitrile solution be made in every lml containing about
The solution of 1.5mg.
The preparation of reference substance solution: Gamithromycin reference substance is taken, is measured in the same method.
Instrument precision measuring method: taking reference substance solution, and 10 μ l of sample volume is repeated sample introduction 6 times, with retention time, peak face
Product calculates relative standard deviation (RSD).As a result 2 be see the table below.
The instrument precision test result of 2 Gamithromycin assay of table
| Number | 1 | 2 | 3 | 4 | 5 | 6 | Mean value | RSD (%) |
| Retention time (min) | 18.364 | 18.374 | 18.379 | 18.388 | 18.394 | 18.398 | 18.383 | 0.07 |
| Peak area (mAU*s) | 1777.4 | 1788.7 | 1787.7 | 1773.4 | 1788.4 | 1769.1 | 1780.8 | 0.48 |
Conclusion: the above Precision test result show the RSD of contrast solution main peak retention time less than 1.0%, peak area
RSD less than 2.0%, illustrate that this method instrument precision is good.
Method precision measuring method: taking 6 parts of test solution, 10 μ l of sample volume, calculates content by external standard method.Containing measurement
Determine result and calculates relative standard deviation (RSD).As a result 3 be see the table below.
The method precision test result of 3 Gamithromycin assay of table
| Number | 1 | 2 | 3 | 4 | 5 | 6 | Mean value | RSD (%) |
| Content (%) | 101.74 | 100.94 | 101.73 | 100.25 | 100.18 | 101.53 | 101.06 | 0.71 |
Conclusion: the above Precision test result shows that the method precision RSD of test sample assay less than 2.0%, is said
The precision of bright this method is good.
Experimental example 3: the linear test of Gamithromycin content detection
Chromatographic condition and system suitability: Agilengt1260 high performance liquid chromatograph DAD detector, Ultimate
Polar-RP, 5 μm, 4.6 × 250mm chromatographic column；Using acetonitrile-water-liquor ammoniae fortis of volume ratio 65:35:0.1 as mobile phase；Inspection
Survey wavelength is 210nm；Flow velocity is 1.0ml/min；Column temperature is 40 DEG C.Number of theoretical plate should be not less than by the calculating of Gamithromycin peak
5000。
Sample preparation: taking Gamithromycin reference substance appropriate, and by 1 method of test example, it is dense that difference containing Gamithromycin is respectively prepared
The solution of degree injects liquid chromatograph, records chromatogram.Testing result see the table below 4.Using reference substance concentration C as abscissa, peak face
Product A is ordinate, draws curve, sees attached drawing 3.
The testing result and regression equation of 4 various concentration Gamithromycin of table
Conclusion: the above result shows that, Gamithromycin is in 0.9mg/ml~2.3mg/ml concentration range, linear equation y
=1066.5x-17.4, correlation coefficient r=0.9999, linear relationship are good.
Experimental example 4: the method accuracy test of Gamithromycin content detection
Chromatographic condition and system suitability: Agilengt1260 high performance liquid chromatograph DAD detector, Ultimate
Polar-RP, 5 μm, 4.6 × 250mm chromatographic column；Using acetonitrile-water-liquor ammoniae fortis of volume ratio 65:35:0.1 as mobile phase；Inspection
Survey wavelength is 210nm；Flow velocity is 1.0ml/min；Column temperature is 40 DEG C.Number of theoretical plate should be not less than by the calculating of Gamithromycin peak
5000。
Sample preparation: taking Gamithromycin reference substance, by 1 method of test example, prepares 80%, 100%, 120%3 respectively not
With the sample of concentration, 3 parts of each concentration mensuration carries out Gamithromycin recovery test, calculates the rate of recovery.As a result 5 be see the table below.
5 determination of recovery rates result of table
Conclusion: average recovery rate 99.8%, the rate of recovery is in 98.6%~101.1% range, recovery test result
Show to measure Gamithromycin content with this method, the rate of recovery of method is good, and accuracy is high.
Experimental example 5: the Selection experiment of mobile phase
With reference to the detection method of the similar Macrocyclolactone lactone kind medicine azithromycin of Gamithromycin, and most according to Gamithromycin
Big absorbing wavelength, physical and chemical dissolution characteristics, pKa value etc., screening mobile phase is acetonitrile: 0.05mol/l potassium phosphate buffer (is adjusted
Section pH7-8) flow visualizing that provides in=60~80:40~20, with patent CN201310745236 is acetonitrile:
0.025mol/ml dipotassium hydrogen phosphate solution (pH8-8.5)=70:30 is similar, the buffer salt component dosage in the flow visualizing
It is larger, find that chromatographic column and the detector of high performance liquid chromatograph etc. will appear precipitation problem, Jin Erying when actually detected
The problems such as ringing detection data stability or instrument and equipment caused to block.Screening is optimized by test of many times, selects acetonitrile-
Water-liquor ammoniae fortis is the system of mobile phase, and acetonitrile-water-liquor ammoniae fortis that preferred volume ratio is 65:35:0.1 is flowing
Phase；By the methodology validation of above-mentioned experimental example, the accuracy, operation possibility of this method are confirmed.
Experimental example 6: the Selection experiment of chromatographic column
Chromatographic condition and system suitability: using volume ratio for 65:35:0.1 acetonitrile-water-liquor ammoniae fortis as stream
Dynamic phase；Detection wavelength is 210nm；Flow velocity is 1.0ml/min；Column temperature is 40 DEG C.Number of theoretical plate should not by the calculating of Gamithromycin peak
Lower than 5000.
Sample preparation: pressing 1 method of test example, prepares test solution, and precision measures 10 μ l and injects liquid chromatograph, uses
Different chromatography post detections record chromatogram.Investigation the results are shown in Table 6.
The investigation result of the different chromatographic columns of table 6
Conclusion: the above result shows that, using the Polar-RPC18 chromatographic column of Ultimate brand, detect Gamithromycin sample
When product, peak shape symmetry is closer to 1, and peak shape is more preferably.
Experimental example 7: the Selection experiment of dilution
Chromatographic condition and system suitability: Agilengt1260 high performance liquid chromatograph DAD detector, Ultimate
Polar-RP, 5 μm, 4.6 × 250mm chromatographic column；Using volume ratio for 65:35:0.1 acetonitrile-water-liquor ammoniae fortis as flowing
Phase；Detection wavelength is 210nm；Flow velocity is 1.0ml/min；Column temperature is 40 DEG C.Number of theoretical plate should not be low by the calculating of Gamithromycin peak
In 5000.
Sample preparation: 1 method of test example is pressed, selects 65% acetonitrile water (test solution 1) and 65% acetonitrile water-respectively
0.1% liquor ammoniae fortis (test solution 2) is used as dilution, test solution 1 and test solution 2 is prepared, respectively at 0,4,8
Hour, accurate each 10 μ l of solution of measurement injected liquid chromatograph, recorded chromatogram, stability of the investigation solution in 8 hours.It examines
It examines and the results are shown in Table 7,8.
The investigation result of 7 test solution of table, 1 stable content
| Time (h) | 0 | 4 | 8 |
| Indicate content % | 101.74 | 102.13 | 101.54 |
| Variable quantity % | / | 0.39 | -0.20 |
The investigation result of 8 test solution of table, 2 stable content
| Time (h) | 0 | 4 | 8 |
| Indicate content % | 100.16 | 98.53 | 97.01 |
| Variable quantity % | / | -1.63 | -3.15 |
Conclusion: the above result shows that, 1 changes of contents of test solution has good stability less than 1.0% in 8 hours；For
2 changes of contents of test sample solution is greater than in 2.0%, and stability of solution is bad.Therefore, selection 65% acetonitrile solution of volume ratio is made
For the dilution of test sample dissolution, stability of solution more preferably, more can ensure that the accuracy of testing result.
The present invention carries out analysis detection to Gamithromycin content using high performance liquid chromatography, and external standard method determines sample
Amount has following excellent results compared with the existing technology:
1. using conventional detection apparatus, enterprise and market surpervision department are reduced to the new investment of instrument and equipment, conducive to pushing away
It is wide to use: to select high performance liquid chromatograph, detector is examined using such as Agilent DAD detector, diode array is formulated conventionally
Device or 2998 detector of Waters etc. are surveyed, is that medicine supervision department of reaching often uses detector, is not necessarily to second purchase, detection side
Method is similarly conventional method, does not need testing staff, QC personnel etc. and carries out secondary Training Management.
2. flow visualizing of the present invention is stablized, detection data is reliable: not adding buffering salt, nothing in the flow visualizing
The problem of risk is precipitated, and then avoids flow visualizing and detection data unstable, or needs special detection device；Dilution is excellent
Acetonitrile solution is selected to carry out dissolution measuring samples, the difference with mobile phase is to be not added with liquor ammoniae fortis, it is therefore an objective to reduce dilution
The pH of liquid, the stability of solution of sample, excludes the chromatography generated in chromatogram by solvent effect after utmostly ensuring to dissolve
Peak.
3. detection method of the invention is accurately feasible by methodology validation: the method is easy, specificity, reproducibility,
Precision, linear, accuracy is good, and Gamithromycin purity is good, is not interfered by impurity；Instrument precision and method precision RSD
Respectively less than 1%；Gamithromycin is in 0.9mg/ml~2.3mg/ml concentration range, linear equation y=1066.5x-17.4, phase
Relationship number r=0.9999, linear relationship are good；The rate of recovery is in 98%~101% range, and the rate of recovery of method is good, accuracy
It is high.
4. the present invention by screening chromatographic column, find routine Agilent and Waters chromatographic column, peak shape hangover/it is preceding prolong sternly
Weight, compares by screening, and preferably the Polar-RP C18 chromatographic column of Ultimate brand, chromatographic peak do not prolong before relatively, do not trail,
Peak shape symmetry is good.
Detailed description of the invention
Fig. 1 is the high-efficient liquid phase chromatogram of 1 Gamithromycin reference substance of experimental example.
Fig. 2 is the high-efficient liquid phase chromatogram of 1 Gamithromycin test sample of experimental example.
Fig. 3 is the linear standard curve of 3 Gamithromycin reference substance of experimental example.
Specific embodiment
Present invention will be further explained below with reference to the attached drawings and examples, but not limited to this.In embodiment all raw materials and
Equipment is commercial products.
Embodiment 1:
A kind of detection method of content of Gamithromycin, this method are high performance liquid chromatography, and specific steps include:
Chromatographic condition and system suitability: Polar-RP C18,5 μm, 4.6 × 250mm chromatographic column；With volume ratio
Acetonitrile-water-liquor ammoniae fortis of 65:35:0.1 is mobile phase；Detection wavelength is 210nm；Flow velocity is 1.0ml/min；Column temperature is 40
℃.Number of theoretical plate is calculated by Gamithromycin peak should be not less than 5000；2998 detector of Waters.
The preparation of test sample: taking this product 49.5mg into 50ml volumetric flask, with 65% acetonitrile solution constant volume of volume ratio
To scale, concentration is about 1.0mg/ml.
The preparation of reference substance: taking Gamithromycin reference substance 26.6mg, until in 25ml volumetric flask, with 65% acetonitrile of volume ratio
Aqueous solution is settled to scale, and concentration is about 1.0mg/ml.
Measuring method: it is accurate respectively to measure above-mentioned 10 μ l of solution, liquid chromatograph is injected, chromatogram is recorded.By external standard method with
Calculated by peak area.
In reference substance chromatogram, the number of theoretical plate of Gamithromycin chromatographic peak is 10476；In sample chromatogram figure, add rice mould
The number of theoretical plate of plain color spectral peak is 10751, is all satisfied in system suitability requirement.
Reference substance peak area is 1674991, and test sample peak area is 1554642.
Embodiment 2:
A kind of detection method of content of Gamithromycin, this method are high performance liquid chromatography, and specific steps include:
Chromatographic condition and system suitability: Polar-RP C18,5 μm, 4.6 × 250mm chromatographic column；With volume ratio
Acetonitrile-water-liquor ammoniae fortis of 70:30:0.1 is mobile phase；Detection wavelength is 210nm；Flow velocity is 1.2ml/min；Column temperature is 35
℃.Number of theoretical plate is calculated by Gamithromycin peak should be not less than 5000；Agilent 1260DAD detector.
The preparation of test sample: taking this product 49.3mg into 50ml volumetric flask, with 65% acetonitrile solution constant volume of volume ratio
To scale, concentration is about 1.0mg/ml.
The preparation of reference substance: taking Gamithromycin reference substance 25.8mg, until in 25ml volumetric flask, with 65% acetonitrile of volume ratio
Aqueous solution is settled to scale.
Measuring method: it is accurate respectively to measure above-mentioned 10 μ l of solution, liquid chromatograph is injected, chromatogram is recorded.By external standard method with
Calculated by peak area.
Reference substance peak area is 1747.1, and test sample peak area is 1669.1.
Claims (10)
1. a kind of detection method of content of Gamithromycin, this method are high performance liquid chromatography, which is characterized in that comprising steps of
Chromatographic condition and system suitability: being filler with octadecylsilane chemically bonded silica；With volume ratio 60-75:25-
Acetonitrile-water-liquor ammoniae fortis of 40:0.1 is mobile phase, and survey wavelength is 208nm-220nm；Flow velocity is 0.8ml/min-1.2ml/
min；Column temperature is 30 DEG C -40 DEG C；Number of theoretical plate is calculated by Gamithromycin peak should be not less than 5000；
The preparation of test sample: taking Gamithromycin accurately weighed, is quantitatively diluted and is made in every lml containing 0.5- with acetonitrile solution
The solution of 1.5mg；
The preparation of reference substance: taking Gamithromycin reference substance, ibid the preparation method preparation of test sample；
Measuring method: it is accurate respectively to measure above-mentioned 10 μ l of solution, liquid chromatograph is injected, chromatogram is recorded；By external standard method with peak face
Product calculate to get.
2. the detection method of content of Gamithromycin as described in claim 1, which is characterized in that instrument selection high performance liquid chromatography
2998 detector of instrument Agilent DAD detector or Waters.
3. the detection method of content of Gamithromycin as described in claim 1, which is characterized in that chromatographic column is Polar-RP C18
Chromatographic column, peak shape are preferable；The Polar-RP C18 chromatographic column of further preferred Ultimate brand.
4. the detection method of content of Gamithromycin as described in claim 1, which is characterized in that mobile phase is volume ratio 65:35:
0.1 acetonitrile-water-liquor ammoniae fortis.
5. the detection method of content of Gamithromycin as described in claim 1, which is characterized in that Detection wavelength 210nm.
6. the detection method of content of Gamithromycin as described in claim 1, which is characterized in that flow velocity 1.0ml/min.
7. the detection method of content of Gamithromycin as described in claim 1, which is characterized in that column temperature is 40 DEG C.
8. the detection method of content of Gamithromycin as described in claim 1, which is characterized in that in the preparation of the test sample,
Dilution acetonitrile solution preferred volume ratio is 60%-75%, and further preferred volume ratio is 65%.
9. the detection method of content of Gamithromycin as described in claim 1, which is characterized in that in the preparation of the test sample,
After dilution acetonitrile solution dissolves measuring samples, Gamithromycin sample concentration is 1.0mg/ml.
10. the detection method of content of Gamithromycin as described in claim 1, which is characterized in that step includes:
Chromatographic condition and system suitability: being filler with octadecylsilane chemically bonded silica；With volume ratio 65:35:0.1
Acetonitrile-water-liquor ammoniae fortis be mobile phase；Detection wavelength is 210nm；Flow velocity is 1.0ml/min；Column temperature is 40 DEG C；Theoretical plate
Number is calculated by Gamithromycin peak should be not less than 5000；
The preparation of test solution: taking Gamithromycin accurately weighed, is quantitatively diluted and is made with 65% acetonitrile solution of volume ratio
Solution in every lml containing about 0.5-1.5mg；
The preparation of reference substance solution: taking Gamithromycin reference substance, ibid the preparation method preparation of test sample；
Measuring method: it is accurate respectively to measure above-mentioned 10 μ l of solution, liquid chromatograph is injected, chromatogram is recorded；By external standard method with peak face
Product calculate to get.
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