CN112924602B - Method for detecting lincomycin impurity F in lincomycin hydrochloride injection by high performance liquid chromatography-evaporative light method - Google Patents
Method for detecting lincomycin impurity F in lincomycin hydrochloride injection by high performance liquid chromatography-evaporative light method Download PDFInfo
- Publication number
- CN112924602B CN112924602B CN202110334991.7A CN202110334991A CN112924602B CN 112924602 B CN112924602 B CN 112924602B CN 202110334991 A CN202110334991 A CN 202110334991A CN 112924602 B CN112924602 B CN 112924602B
- Authority
- CN
- China
- Prior art keywords
- lincomycin
- impurity
- high performance
- performance liquid
- liquid chromatography
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- 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
-
- 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
- G01N30/62—Detectors specially adapted therefor
- G01N30/74—Optical detectors
-
- 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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Investigating Or Analysing Biological Materials (AREA)
Abstract
The invention relates to a method for detecting lincomycin impurity F in lincomycin hydrochloride injection by a high performance liquid chromatography-evaporative light method, wherein a mobile phase A of the method is a trifluoroacetic acid-heptafluorobutyric anhydride solution with the mass fraction of 0.01%, wherein the concentration of the heptafluorobutyric anhydride is 10mmol/L, and a mobile phase B is a methanol solution; the volume ratio of the two is 65. The method can realize accurate qualitative and quantitative detection of the lincomycin impurity F, and provides an effective and reliable detection means for product detection of the lincomycin hydrochloride injection.
Description
Technical Field
The invention relates to the field of pharmaceutical preparations, in particular to a method for detecting lincomycin impurity F in lincomycin hydrochloride injection by a high performance liquid chromatography-evaporative light method.
Background
Lincomycin hydrochloride is available in the form of tablet, capsule, eye drop, ear drop, injection, ointment, etc. Is used as bacteriostatic agent. Can be used for treating respiratory tract infection, skin soft tissue infection, female genital tract infection, pelvic infection and abdominal infection caused by sensitive staphylococcus, streptococcus pneumoniae and anaerobe.
In lincomycin hydrochloride injection, the following impurities may be present:
lincomycin impurity F, chemical name: 6-amino-6,8-dideoxy-1-thio-D-erythro- α -D-galactose-octapyranoside, structural formula:
lincomycin impurity F belongs to degradation impurities and is sensitive to temperature and illumination, and the lincomycin impurity F can be obviously increased in the long-term storage process. Impurities are main factors influencing the quality and the medication safety of the medicine, so that the accurate control of the content of the impurities is a necessary means for ensuring the quality of the medicine and the medication safety of patients.
The sensitivity of a detection method is the lowest detection limit for a detection target, and in a quantitative detection method, the sensitivity is an important index for judging whether the detection method is effective or not.
At present, the quality standard of lincomycin hydrochloride injection is recorded in pharmacopoeias of China, america, japan, british and other countries and countries, wherein the 'British pharmacopoeia' of 2019 edition, the 'United states pharmacopoeia' of 42 edition and the 'Japanese medicine local prescription' of 17 edition do not stipulate the detection method of related substances of lincomycin hydrochloride injection, and the 'Chinese pharmacopoeia' of 2020 edition adopts a high performance liquid chromatograph ultraviolet detection method to detect the related substances of lincomycin hydrochloride injection. With the stricter and stricter requirements of the national drug policy, the quality of the drug needs to be improved and broken through continuously. At present, the latest 2020 edition of Chinese pharmacopoeia adopts a high performance liquid chromatograph ultraviolet detection method to detect related substances of lincomycin hydrochloride injection, the separation degree is poor, lincomycin impurity F cannot be completely separated from chromatographic peaks of other impurities by adopting the Chinese pharmacopoeia method to detect the lincomycin impurity F, the impurity F cannot be accurately identified and detected, the limit of the impurity F cannot be clearly defined, and qualitative and quantitative detection on the lincomycin impurity F cannot be accurately carried out, so that the product quality cannot be comprehensively ensured.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for detecting impurities in lincomycin hydrochloride injection by a high performance liquid chromatography-evaporative light method.
The technical scheme for solving the technical problems is as follows: a method for detecting lincomycin impurity F in lincomycin hydrochloride injection by a high performance liquid chromatography-evaporative light method is characterized in that,
the mobile phase of the high performance liquid chromatography is that the mobile phase A is trifluoroacetic acid-heptafluorobutyric anhydride solution with the mass fraction of 0.01 percent, wherein the concentration of the heptafluorobutyric anhydride is 10mmol/L, and the mobile phase B is methanol solution; the volume ratio of the two is 65;
the column temperature of the high performance liquid chromatography-evaporative light method is 25-40 ℃, the flow rate is 0.7-1.5ml/mi, and the temperature of a drift tube of an evaporative light scattering detector is 50-70 ℃; the flow rate of the carrier gas is 1.5-3.0L/min.
The method has the beneficial effects that chromatographic peaks of lincomycin impurity F can be effectively and completely separated through the detection conditions; for the column temperature, when the column temperature is higher than 40 ℃, other impurities in the lincomycin hydrochloride injection interfere the detection of the impurity F, partial overlapping phenomenon occurs on the chromatographic peaks of the impurities, and the separation degree does not meet the requirement; the high proportion of methanol in the mobile phase can prevent the peak emergence time of each chromatographic peak in the sample from being seriously delayed, and the detection efficiency is improved when the detection time is shortened.
According to the invention, the addition of heptafluorobutyric anhydride in the mobile phase of the impurity F is beneficial to improving the chromatographic peak shape of the impurity F and improving the symmetry of the chromatographic peak.
Further, the column temperature of the high performance liquid chromatography-evaporative light method is 30 ℃, and the flow rate is 0.9ml/min; the temperature of the drift tube of the evaporative light scattering detector is 50 ℃, and the carrier gas flow is 1.5L/min.
Further, the sensitivity for detecting lincomycin impurity F is 0.1%.
Furthermore, the chromatographic column of the high performance liquid chromatography-evaporative light method is an octadecylsilane chemically bonded silica chromatographic column.
Further, the carrier gas used for the detection by the high performance liquid chromatography-evaporative light method is nitrogen.
Further, the method comprises the following steps:
s1, preparation of a sample: taking lincomycin hydrochloride injection, and diluting the lincomycin hydrochloride injection by using a mixed solution of methanol and water with the volume ratio of 20;
s2, preparing a standard solution: taking a lincomycin impurity F standard substance, adding a mixed solution of methanol and water with the volume ratio of 20;
s3, analyzing and detecting a sample: detecting the sample to be detected in the step S1 by using the high performance liquid chromatography-evaporative light method, and obtaining a chromatogram map of the sample to be detected;
s4, drawing a standard curve: detecting the standard solution of the lincomycin impurity F with each concentration gradient in the step S2 by adopting the high performance liquid chromatography-evaporative light method in the step S3 to respectively obtain chromatograms corresponding to the standard solution of the lincomycin impurity F with each concentration gradient; drawing a standard curve according to the lincomycin impurity F standard substance solutions with different concentration gradients and peak areas corresponding to the lincomycin impurity F standard substance solutions to obtain a lincomycin impurity F standard equation;
s5, carrying out qualitative analysis on the sample: comparing the chromatogram of the sample to be detected in the step S3 with the peak appearance time of the chromatogram of the standard solution of any concentration gradient of lincomycin impurity F in the step S4, and identifying the chromatographic peak at the same peak appearance time as the chromatogram of the lincomycin impurity F standard solution of any concentration gradient, wherein the chromatographic peak is the chromatographic peak of the lincomycin impurity F;
s6, carrying out quantitative analysis on the sample: substituting the peak area of the chromatographic peak of the lincomycin impurity F in the chromatogram of the solution to be detected obtained in the step S5 into the lincomycin impurity F standard equation in the step S4 to obtain the content of the lincomycin impurity F in the sample to be detected.
Further, in the step S1, 1.7ml of lincomycin hydrochloride injection is taken and placed in a 50ml volumetric flask, and a mixed solution of methanol and water with a volume ratio of 20.
Further, in the step S1, the concentration gradient of the standard product of the lincomycin impurity F for quantitative dilution is 50ug/mL, 100ug/mL and 150ug/mL.
Further, in the step S3 and the step S4, the sample injection amount of the sample to be tested and the standard solution of the lincomycin impurity F is 10 μ l.
According to the method for detecting the lincomycin impurity F in the lincomycin hydrochloride injection by the high performance liquid chromatography-evaporative light method, the mobile phase suitable for the lincomycin impurity F is arranged, and the chromatographic conditions such as the appropriate column temperature, the appropriate flow rate and the like are matched, so that the chromatographic peak of the lincomycin impurity F can be completely separated from the chromatographic peaks of other components, the accurate qualitative and quantitative detection of the lincomycin impurity F is realized, and an effective and reliable detection means is provided for the product detection of the lincomycin hydrochloride injection.
Drawings
FIG. 1 is a chromatogram of a lincomycin impurity F standard 2 in example 1 of the invention;
FIG. 2 is a chromatogram of a first set of solutions of samples to be tested in example 1 of the present invention;
FIG. 3 is a standard curve of lincomycin impurity F in example 1 of the present invention;
fig. 4 is a chromatogram of a second group of sample solutions to be tested in embodiment 2 of the present invention;
FIG. 5 is a chromatogram of a lincomycin impurity F standard sample detected by a high performance liquid chromatograph in an ultraviolet manner in example 3 of the invention;
fig. 6 is a chromatogram of a third set of solutions of samples to be tested, which are detected by using a high performance liquid chromatograph in ultraviolet in example 4 of the present invention.
Detailed Description
The principles and features of this invention are described below in conjunction with the following drawings, which are set forth by way of illustration only and are not intended to limit the scope of the invention.
The method for detecting the lincomycin impurity F in the lincomycin hydrochloride injection by the high performance liquid chromatography-evaporative light method can qualitatively and quantitatively detect the lincomycin impurity F in the lincomycin hydrochloride injection. The invention will be verified for the effectiveness of the method by the following examples.
In the following embodiments, the sample solutions to be tested used are a first group of samples to be tested, a second group of samples to be tested, and a third group of samples to be tested, respectively; the preparation method of the first group and the second group of samples to be detected comprises the steps of taking 1.7ml of lincomycin hydrochloride injection, placing the lincomycin hydrochloride injection into a 50ml volumetric flask, adding a mixed solution of methanol and water with the volume ratio of 20 to dissolve the lincomycin hydrochloride injection and quantitatively diluting the lincomycin hydrochloride injection to a scale, and obtaining a sample solution to be detected with the concentration of 10.2 mg/ml; the third group of samples to be tested is prepared by taking 0.05mol/L borax solution (pH value is adjusted to 5.0 by 85% phosphoric acid solution) -methanol-acetonitrile (67-33) as a mobile phase, taking lincomycin hydrochloride injection, and diluting with the mobile phase to prepare a solution containing about 4mg of lincomycin in each 1ml as a test solution. The sample lot number for the above sample was 20061503.
Example 1
The detection method is adopted to detect lincomycin impurity F in the lincomycin hydrochloride injection, wherein the chromatographic condition of detection is that the temperature of a drift tube of an evaporative light scattering detector is 50 ℃; the carrier gas flow is 1.5L/min; the column temperature is 30 ℃; the flow rate was 0.9ml/min.
The detection data of each concentration gradient of the lincomycin impurity F standard are shown in Table 1:
TABLE 1 detection data for each concentration gradient of lincomycin impurity F standard
Wherein, the chromatogram of the lincomycin impurity F standard 2 is shown in figure 1, and the chromatogram of the sample solution to be detected is shown in figure 2.
And drawing a standard curve of the lincomycin impurity F standard according to the detection data such as the concentration, the peak area and the like of the standard, wherein the standard curve is shown in figure 3. The standard curve equation is that y =1.4481x +14.758 2 ＝0.9996。
Substituting the peak area of the sample to be measured, which is measured in the embodiment, into the standard curve equation, and calculating to obtain the content percentage of lincomycin impurity F, wherein the specific numerical values are shown in Table 2:
TABLE 2 percentage of lincomycin impurity F in the first set of samples to be tested
In this embodiment, the lincomycin impurity F standard is detected under the preferable chromatographic conditions in the method of the present invention, and the peak-off time of the lincomycin impurity F standard is 5.582min as can be known from the standard chromatogram of fig. 1; comparing the chromatogram of the first group of samples to be detected in fig. 2 with the chromatogram of the standard substance in fig. 1, the peak with the peak emergence time of 5.539min is the lincomycin impurity F, so the method can qualitatively detect the lincomycin impurity F contained in the lincomycin hydrochloride injection. Meanwhile, as is apparent from fig. 2, the separation degree of lincomycin impurity F reaches 23.14, and the method has good separation degree.
In this embodiment, the relationship between the peak area and the content of lincomycin impurity F can be obtained by the standard curve equation of the standard, and the peak area of the first group of samples to be measured is substituted into the standard curve equation, so that the lincomycin impurity F content in the group of samples is 61ug/mL, accounting for 0.60%.
And meanwhile, according to the chromatogram, the concentration of the lincomycin impurity F when the signal-to-noise ratio of the chromatogram of the lincomycin impurity F reference solution is about 3 is taken as the minimum detection concentration of the lincomycin impurity F, and the percentage content of the lincomycin impurity F in the lincomycin hydrochloride injection is converted according to the specification and the dilution concentration of a lincomycin injection sample.
The detection sensitivity for detecting the lincomycin impurity F is that the lincomycin impurity F with the mass percent of 0.1% can be detected.
Example 2
The detection method is adopted to detect lincomycin impurity F in the lincomycin hydrochloride injection, wherein the chromatographic condition of detection is that the temperature of a drift tube of an evaporative light scattering detector is 60 ℃; the carrier gas flow is 2.2L/min; the column temperature was 35 ℃; the flow rate was 1.2ml/min.
The chromatogram of the lincomycin impurity F in the second group of sample solutions to be detected is shown in figure 4.
By adopting the chromatographic conditions in the embodiment, the detected lincomycin impurity F has the peak time of 5.546min and the separation degree of 23.77, and the lincomycin impurity F can still be detected qualitatively and quantitatively by adopting the method.
Example 3
And detecting the lincomycin impurity F standard substance and a third group of sample solution to be detected by adopting a high performance liquid chromatograph ultraviolet detection method recorded in the Chinese pharmacopoeia in the prior art.
Wherein, the high performance liquid chromatograph ultraviolet detection has the chromatographic condition that the detection wavelength is 214nm; the column temperature is 30 ℃; the flow rate was 0.5ml/min.
The chromatogram of the lincomycin impurity F standard substance detected by ultraviolet rays of the high performance liquid chromatograph is shown in fig. 5, and the chromatogram of the third group of sample solutions to be detected is shown in fig. 6.
In the embodiment, the chromatogram 5 of the lincomycin impurity F standard shows that the peak-off time is 6.155min, the retention time is too short, and the retention time is partially overlapped with the diluent peak; in the chromatogram 6 of the third group of sample solutions to be detected, two chromatographic peaks appearing under 5.318min and 6.163min are partially overlapped, the separation degree is only 1.34, lincomycin impurity F cannot be completely separated from the chromatographic peaks of other impurities, so that the impurity F cannot be accurately identified and detected, the limit of the impurity cannot be clearly defined, the lincomycin impurity F cannot be accurately qualitatively detected, and the accurate quantitative detection cannot be further performed.
In examples 1 to 3, the comparison of the separation ratios of lincomycin impurity F detected by the detection method of the present patent and the detection method of the prior art is shown in Table 3:
TABLE 3 degrees of separation of the detection methods of examples 1 to 3
The comparison in table 3 shows that the method for detecting lincomycin impurity F has good separation degree, the separation degree is poor by adopting the existing method, and the method does not meet the standard requirement of Chinese pharmacopoeia.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (8)
1. A method for detecting lincomycin impurity F in lincomycin hydrochloride injection by a high performance liquid chromatography-evaporative light method is characterized in that,
the mobile phase of the high performance liquid chromatography is that the mobile phase A is a trifluoroacetic acid-heptafluorobutyric anhydride solution with the mass fraction of 0.01 percent, wherein the concentration of the heptafluorobutyric anhydride is 10mmol/L, and the mobile phase B is a methanol solution; the volume ratio of the two is 65;
the column temperature of the high performance liquid chromatography-evaporative light method is 25-40 ℃, the flow rate is 0.7-1.5ml/min, and the temperature of a drift tube of an evaporative light scattering detector is 50-70 ℃; the carrier gas flow is 1.5-3.0L/min;
the chromatographic column of the high performance liquid chromatography-evaporative light method is an octadecylsilane chemically bonded silica chromatographic column.
2. The method for detecting lincomycin impurity F in lincomycin hydrochloride injection by the high performance liquid chromatography-evaporative light method as claimed in claim 1,
the column temperature of the high performance liquid chromatography-evaporative light method is 30 ℃, and the flow rate is 0.9ml/min; the temperature of the drift tube of the evaporative light scattering detector is 50 ℃, and the carrier gas flow is 1.5L/min.
3. The method for detecting lincomycin impurity F in lincomycin hydrochloride injection by using the high performance liquid chromatography-evaporative light method as claimed in claim 2, wherein the detection sensitivity for detecting the lincomycin impurity F is 0.1%.
4. The method for detecting lincomycin impurity F in lincomycin hydrochloride injection by the high performance liquid chromatography-evaporative light method as claimed in claim 1, wherein a carrier gas used for the detection by the high performance liquid chromatography-evaporative light method is nitrogen.
5. The method for detecting lincomycin impurity F in lincomycin hydrochloride injection by the high performance liquid chromatography-evaporative light method as claimed in any one of claims 1 to 4,
the method comprises the following steps:
s1, preparation of a sample: taking lincomycin hydrochloride injection, and diluting the lincomycin hydrochloride injection by using a mixed solution of methanol and water with the volume ratio of 20;
s2, preparing a standard solution: taking a lincomycin impurity F standard substance, adding a mixed solution of methanol and water with the volume ratio of 20;
s3, analyzing and detecting a sample: detecting the sample to be detected in the step S1 by the high performance liquid chromatography-evaporative light method, and obtaining a chromatogram of the sample to be detected;
s4, drawing a standard curve: detecting the standard solution of the lincomycin impurity F with each concentration gradient in the step S2 by adopting the high performance liquid chromatography-evaporative light method in the step S3 to respectively obtain chromatograms corresponding to the standard solution of the lincomycin impurity F with each concentration gradient; drawing a standard curve according to the lincomycin impurity F standard substance solutions with different concentration gradients and peak areas corresponding to the lincomycin impurity F standard substance solutions to obtain a lincomycin impurity F standard equation;
s5, carrying out qualitative analysis on the sample: comparing the chromatogram of the sample to be detected in the step S3 with the peak appearance time of the chromatogram of the standard solution of any concentration gradient of lincomycin impurity F in the step S4, and identifying the chromatographic peak at the same peak appearance time as the chromatogram of the lincomycin impurity F standard solution of any concentration gradient, wherein the chromatographic peak is the chromatographic peak of the lincomycin impurity F;
s6, carrying out quantitative analysis on the sample: substituting the peak area of the chromatographic peak of the lincomycin impurity F in the chromatogram of the solution to be detected obtained in the step S5 into the lincomycin impurity F standard equation in the step S4 to obtain the content of the lincomycin impurity F in the sample to be detected.
6. The method for detecting lincomycin impurity F in the lincomycin hydrochloride injection by the high performance liquid chromatography-evaporative light method as claimed in claim 5,
in the step S1, 1.7ml of lincomycin hydrochloride injection is taken and placed in a 50ml volumetric flask, and a mixed solution of methanol and water with the volume ratio of 20.
7. The method for detecting lincomycin impurity F in the lincomycin hydrochloride injection by the high performance liquid chromatography-evaporative light method as claimed in claim 5,
in the step S2, the concentration gradient of the standard product of the lincomycin impurity F for quantitative dilution is 50ug/mL, 100ug/mL and 150ug/mL.
8. The method for detecting lincomycin impurity F in the lincomycin hydrochloride injection by the high performance liquid chromatography-evaporative light method as claimed in claim 5,
in the step S3 and the step S4, the sample volume of the sample to be detected and the standard solution of the lincomycin impurity F is 10 μ l.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110334991.7A CN112924602B (en) | 2021-03-29 | 2021-03-29 | Method for detecting lincomycin impurity F in lincomycin hydrochloride injection by high performance liquid chromatography-evaporative light method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110334991.7A CN112924602B (en) | 2021-03-29 | 2021-03-29 | Method for detecting lincomycin impurity F in lincomycin hydrochloride injection by high performance liquid chromatography-evaporative light method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN112924602A CN112924602A (en) | 2021-06-08 |
| CN112924602B true CN112924602B (en) | 2023-03-28 |
Family
ID=76176435
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110334991.7A Active CN112924602B (en) | 2021-03-29 | 2021-03-29 | Method for detecting lincomycin impurity F in lincomycin hydrochloride injection by high performance liquid chromatography-evaporative light method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112924602B (en) |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103487518B (en) * | 2013-09-02 | 2015-03-18 | 成都百裕科技制药有限公司 | Impurity detection method and content determination method for clindamycin hydrochloride for injection |
| WO2016205172A1 (en) * | 2015-06-15 | 2016-12-22 | Banner Life Sciences Llc | Soft lozenges comprising corticosteroids |
| CN108226324B (en) * | 2017-12-14 | 2021-01-12 | 兆科（广州）眼科药物有限公司 | Impurity control method of clindamycin hydrochloride |
-
2021
- 2021-03-29 CN CN202110334991.7A patent/CN112924602B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN112924602A (en) | 2021-06-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104914185A (en) | HPLC method for measuring related substances in Favipiravir | |
| CN109060973B (en) | Method for detecting ethylenediamine in lipoic acid injection | |
| CN102798678A (en) | Detection method and content determining method of sodium calcium edetate in pantoprazole sodium for injecting | |
| CN112924601B (en) | Method for detecting lincomycin impurity E in lincomycin hydrochloride injection by high performance liquid chromatography-evaporative light method | |
| CN113125611B (en) | Method for detecting content of impurity 6-formyl pterin folic acid | |
| CN106033079B (en) | Method for detecting related substance imidazole in starting material F of dabigatran etexilate mesylate | |
| CN106525994B (en) | Method for determining related substances of paracetamol and tramadol capsule | |
| CN112924602B (en) | Method for detecting lincomycin impurity F in lincomycin hydrochloride injection by high performance liquid chromatography-evaporative light method | |
| CN111551645A (en) | Method for detecting hydroxychloroquine sulfate related substances and application thereof | |
| CN114839287B (en) | Method for detecting sodium myristate in miboplatin | |
| CN115480020A (en) | Method for measuring substances related to propodoiodoammonium | |
| CN115308335A (en) | Method for detecting blood concentration of aripiprazole | |
| CN111044641B (en) | Hydroxyurea and detection method and application of preparation thereof | |
| CN112666278A (en) | Limit detection method for strychnine in Huatuo reconstruction pills | |
| CN113514589A (en) | High performance liquid chromatography analysis method of stannous glucoheptonate related substance for injection | |
| CN111257458B (en) | Detection method and application of 3-quinuclidinone hydrochloride | |
| CN113030321B (en) | Fingerprint construction method and application of evodia rutaecarpa and asarum preparation | |
| CN117890496B (en) | Method for detecting related substances of compound preparation of novel oral solution of guaifenesin | |
| CN115078576B (en) | Analytical method for related substances of paracetamol and dihydrocodeine tablet | |
| CN115166083B (en) | Method for detecting fosfomycin trometamol related substances and application thereof | |
| CN112394112B (en) | Method for detecting content of hydroxychloroquine oxynitride impurities in hydroxychloroquine sulfate | |
| CN110907548B (en) | Method for detecting biapenem and/or related substances | |
| CN117890519A (en) | Method for determining purity of fluorine-18F marked PSMA radioactive drug by high performance liquid chromatography | |
| CN116482257A (en) | Analysis method for soluble detection of dopa-hydrazine preparation | |
| CN116046950A (en) | Method for detecting 5 impurities in abiraterone acetate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |