CN114965791B - Method for measuring residue in pleshafu by headspace gas chromatography - Google Patents
Method for measuring residue in pleshafu by headspace gas chromatography Download PDFInfo
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- CN114965791B CN114965791B CN202210667823.4A CN202210667823A CN114965791B CN 114965791 B CN114965791 B CN 114965791B CN 202210667823 A CN202210667823 A CN 202210667823A CN 114965791 B CN114965791 B CN 114965791B
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- 238000000034 method Methods 0.000 title claims abstract description 20
- 238000003988 headspace gas chromatography Methods 0.000 title claims abstract description 11
- JGFZNNIVVJXRND-UHFFFAOYSA-N N,N-Diisopropylethylamine (DIPEA) Chemical compound CCN(C(C)C)C(C)C JGFZNNIVVJXRND-UHFFFAOYSA-N 0.000 claims abstract description 82
- 239000000523 sample Substances 0.000 claims abstract description 19
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000012488 sample solution Substances 0.000 claims abstract description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000010453 quartz Substances 0.000 claims abstract description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 7
- 238000005259 measurement Methods 0.000 claims abstract description 6
- 239000012159 carrier gas Substances 0.000 claims abstract description 4
- 238000001514 detection method Methods 0.000 claims abstract description 4
- 230000035945 sensitivity Effects 0.000 claims abstract description 4
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 28
- 239000013558 reference substance Substances 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 6
- 239000011248 coating agent Substances 0.000 claims description 5
- 238000000576 coating method Methods 0.000 claims description 5
- 238000012360 testing method Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 4
- 229910052734 helium Inorganic materials 0.000 claims description 3
- 239000001307 helium Substances 0.000 claims description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 3
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 2
- 238000004587 chromatography analysis Methods 0.000 claims 1
- 239000012224 working solution Substances 0.000 abstract description 8
- 238000002347 injection Methods 0.000 abstract description 5
- 239000007924 injection Substances 0.000 abstract description 5
- 238000011084 recovery Methods 0.000 abstract description 4
- 239000002904 solvent Substances 0.000 abstract description 4
- 239000012085 test solution Substances 0.000 abstract description 3
- 238000010812 external standard method Methods 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract description 2
- 101100283966 Pectobacterium carotovorum subsp. carotovorum outN gene Proteins 0.000 abstract 1
- 238000009472 formulation Methods 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 13
- 208000015914 Non-Hodgkin lymphomas Diseases 0.000 description 5
- 206010035226 Plasma cell myeloma Diseases 0.000 description 5
- 102000004269 Granulocyte Colony-Stimulating Factor Human genes 0.000 description 4
- 108010017080 Granulocyte Colony-Stimulating Factor Proteins 0.000 description 4
- 239000011550 stock solution Substances 0.000 description 4
- 210000003958 hematopoietic stem cell Anatomy 0.000 description 3
- 201000000050 myeloid neoplasm Diseases 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 208000034578 Multiple myelomas Diseases 0.000 description 2
- 238000007865 diluting Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- FSVJFNAIGNNGKK-UHFFFAOYSA-N 2-[cyclohexyl(oxo)methyl]-3,6,7,11b-tetrahydro-1H-pyrazino[2,1-a]isoquinolin-4-one Chemical compound C1C(C2=CC=CC=C2CC2)N2C(=O)CN1C(=O)C1CCCCC1 FSVJFNAIGNNGKK-UHFFFAOYSA-N 0.000 description 1
- 102000019034 Chemokines Human genes 0.000 description 1
- 108010012236 Chemokines Proteins 0.000 description 1
- 206010025323 Lymphomas Diseases 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 239000002576 chemokine receptor CXCR4 antagonist Substances 0.000 description 1
- 239000004205 dimethyl polysiloxane Substances 0.000 description 1
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000012417 linear regression Methods 0.000 description 1
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 229960002957 praziquantel Drugs 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
Classifications
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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
-
- 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
- G01N30/64—Electrical detectors
- G01N30/68—Flame ionisation detectors
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/55—Design of synthesis routes, e.g. reducing the use of auxiliary or protecting groups
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- 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)
- Investigating Or Analysing Biological Materials (AREA)
Abstract
The invention discloses a method for measuring residue in pleshafu by headspace gas chromatographyN,N-a process for diisopropylethylamine comprising: taking outN,NProper diisopropylethylamine and diluted with solvent (DMSO) to 1mLN,NWorking solution of diisopropylethylamine 0.025, mg, simultaneously with the same solvent formulation of pleshafu at a concentration of 25mg/mL as test solution; the chromatographic column for measurement uses quartz capillary column, the initial temperature condition of column temperature box is 40 o C, temperature programming 15 o C per minute, rise to 240 o C, keeping for 2min; at the FID detector 260 o C, the temperature of the sample inlet is 200 o And C, detecting under the chromatographic condition that the split ratio is 5:1 and the carrier gas is nitrogen, taking the sample solution and the working solution, placing the sample solution and the working solution into a sample injection bottle, injecting sample, recording a chromatogram, and calculating by an external standard method. The method has the characteristics of good separation degree of the measurement result, simplicity, rapidness, strong specificity, high sensitivity and the like. The method has good linearity (Y=71398.8817X+4241.1206, R) 2 = 0.9979), the loading recovery was 106%. It is suitable for measuring residue in pleshafuN,NDiisopropylethylamine limit detection.
Description
Technical field:
the invention relates to a method for measuring residual N, N-diisopropylethylamine in pleshafu by using headspace gas chromatography, belonging to the technical field of medicine analysis.
The background technology is as follows:
pleshafu chemical name: 1,1' - [1, 4-benzenedi (methylene) ] di-1, 4,8, 11-tetraazacyclotetradecane.
The chemical structural formula is as follows:
pleshafu, a chemokine CXCR4 receptor antagonist developed by Genzyme corporation of france (purchased from cinnoliavant corporation), was first marketed in the united states at 12 and 15 of 2008 for administration in combination with granulocyte colony-stimulating factor (G-CSF) to promote hematopoietic stem cells into the bloodstream of non-hodgkin lymphoma (NHL) and Multiple Myeloma (MM) patients for collection, followed by autograft; later on in the european union, 7 months 2009, for administration in combination with granulocyte colony-stimulating factor (G-CSF), to promote hematopoietic stem cells into the bloodstream of lymphoma and Multiple Myeloma (MM) patients for collection, followed by autograft; market in japan in 2016, 12, for the promotion of hematopoietic stem cells into the patient's blood stream for collection, followed by autograft. At present, the product is not marketed in China, the original research injection report is produced (NHL, 2018Q2 batch production), 3 raw materials and injection (chemical 3.1 class) are imitated in China to approve clinic (Jiangsu Osaikang pharmaceutical industry, guozhen Yixin pharmaceutical industry, hunan Wuzhou pharmaceutical industry), wherein the pharmacokinetics and the verification clinic of Guozhen Yixin and Hunan Wuzhou are all recruited, the indications are NHL, NHL+MM respectively, and the original research batch postnatal chemical 4 class imitation report is planned.
The invention comprises the following steps:
the invention aims to provide a method for measuring residual N, N-diisopropylethylamine in pleshafu by headspace gas chromatography, which can be used for testing residual N, N-diisopropylethylamine in pleshafu, ensures that the residual N, N-diisopropylethylamine meets limit requirements, and ensures the quality of pleshafu.
A method for measuring residual N, N-diisopropylethylamine in pleshafu by using headspace gas chromatography is characterized in that a quartz capillary chromatographic column is selected, inert gas is used as a gas source, the column adopts a temperature programming mode, a shunting mode and an FID detector, wherein the inert gas can be nitrogen or helium, the length of the quartz capillary chromatographic column is between 30 and 60m, the diameter of the column is between 0.25 and 0.53mm, the thickness of a coating is between 0.25 and 3 mu m, and when the gas source of carrier gas is nitrogen, the temperature programming condition is as follows: the initial temperature is 40-60 ℃, the heating rate is 10-30 ℃/min, the final temperature is 200-280 ℃, the maintaining time is 1-10 min, and the linear speed is 15-50 cm/s. The headspace temperature is 80-150 ℃ and the shaking time is 15-60 minutes.
In some embodiments of the invention, the length of the quartz capillary chromatographic column is between 30m and 60m, the diameter of the column is between 0.25mm and 0.53mm, and the thickness of the coating is between 0.25 mu m and 3 mu m. Wherein the length of the quartz capillary chromatographic column is preferably 30m, the diameter of the column is preferably 0.32mm, and the thickness of the coating is preferably 3 mu m.
In some embodiments of the invention, the carrier gas source is nitrogen or helium, preferably nitrogen.
In some embodiments of the invention, the temperature programmed conditions are: the initial temperature is 40-60 ℃, preferably 40 ℃, the heating rate is 10-30 ℃/min, preferably 15 ℃, the final temperature is 200-280 ℃, preferably 260 ℃, the maintaining time is 1-10 min, preferably 2min, and the linear speed is 15-50 cm/s, preferably 30cm/s.
In some embodiments of the invention, the headspace temperature is 80 to 150 ℃, preferably 110 ℃, and the shaking time is 15 to 60 minutes, preferably 45 minutes.
In some embodiments of the invention, the temperature of the sample inlet is 180-250 ℃, preferably 200 ℃, and the sample is introduced in a split ratio mode, preferably the split ratio is 5:1.
Still further, the present invention provides a method for determining residual N, N-diisopropylethylamine in pleshafu using headspace gas chromatography, comprising the steps of:
(1) Taking a proper amount of pleshafu, dissolving the pleshafu with dimethyl sulfoxide (DMSO), and then fixing the volume with the dimethyl sulfoxide to prepare a sample solution with the concentration of the pleshafu of 25 mg/mL;
(2) Taking a proper amount of N, N-diisopropylethylamine, dissolving with dimethyl sulfoxide (DMSO), and then fixing the volume with the dimethyl sulfoxide to prepare a reference substance solution with the concentration of 0.025mg/mL of N, N-diisopropylethylamine;
(3) Taking N, N-diisopropylethylamine reference substance solution, and a test sample solution of pleshafu, adopting a headspace gas chromatography to determine residual N, N-diisopropylethylamine in the pleshafu, adjusting detection sensitivity to ensure that the peak height of the N, N-diisopropylethylamine in the reference substance solution is obvious, and if the position of the N, N-diisopropylethylamine in the test sample solution of pleshafu has a peak, the peak area of the N, N-diisopropylethylamine is not larger than the peak area of the position of the N, N-diisopropylethylamine working substance solution, wherein a quartz capillary column is adopted as a chromatographic column for determination, the initial column temperature is 40 ℃, the programmed temperature is 15 ℃/min, the temperature is raised to 240 ℃, and the temperature is kept for 2min; the sample inlet temperature is 200 ℃, the split ratio is 5:1, the linear speed is 30cm/s, a FID detector is adopted, the detector temperature is 260 ℃, 1mL of N, N-diisopropylethylamine reference substance solution and pleshafu sample solution are respectively taken and put into a headspace bottle, a cover is tightly pressed, the headspace sample is put into a headspace sample injector, the headspace temperature is set to be 110 ℃, the shaking time is 45 minutes, and sample injection is carried out according to the method.
The method has the characteristics of good separation degree, simplicity, rapidness, strong specificity, high sensitivity and the like. The method has good linearity (Y=71398.8817X+4241.1206, R) 2 = 0.9979), the loading recovery was 106%. The method is suitable for detecting the limit of the residual N, N-diisopropylethylamine in the pleshafu.
Description of the drawings:
FIG. 1 is a gas chromatogram of N, N-diisopropylethylamine control solution.
FIG. 2 gas chromatogram of N, N-diisopropylethylamine control solution added to test solution of pleshafu.
Figure 3 gas chromatograms of test solutions of pleshafu.
The specific embodiment is as follows:
the present invention will be described in further detail with reference to examples below in order to make the objects, technical solutions and advantages of the present method more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
The principle of application of the present invention will be described in detail with reference to examples.
The method for measuring residual N, N-diisopropylethylamine in pleshafu by using headspace gas chromatography in the embodiment of the invention comprises the following steps:
s101: an appropriate amount of N, N-diisopropylethylamine was taken and diluted with solvent (DMSO) to a control solution of 0.025 mg/1 mL of N, N-diisopropylethylamine. Accurately weighing a proper amount of the sample, and diluting the sample into a solution of 25mg of the sample in each 1mL by using a solvent (DMSO), thus obtaining the sample solution.
S102: taking a quartz capillary column (30 m is 0.53mm is 3.0um, a fixing solution is 6% cyanopropylbenzene-94% dimethyl polysiloxane) as a chromatographic column for measurement, wherein the column temperature is kept for 2min at a starting temperature of 40 ℃ and a rate of 15 ℃ per minute to 240 ℃;
s103: detecting under the chromatographic condition that the temperature of an FID detector is 260 ℃, the temperature of a sample inlet is 200 ℃, the split ratio is 5:1, taking a sample solution and working solution to be tested, placing the sample solution and the working solution into a sample injection bottle, the headspace temperature is 110 ℃, the shaking time is 45 minutes, sampling, recording a chromatogram, and calculating by an external standard method.
The principle of application of the present invention will be further described with reference to examples.
(1) Linear investigation
Taking proper amount of N, N-diisopropylethylamine, precisely weighing, preparing a stock solution containing 2500 mug of N, N-diisopropylethylamine in each 1mL by using the solution, obtaining a stock solution A, accurately weighing the stock solution A, and respectively diluting the stock solution A into standard solutions with the concentration of 0.0125mg/mL, 0.02mg/mL, 0.03mg/mL and 0.0375 mg/mL. 1 μl of sample was introduced and peak areas were recorded. The N, N-diisopropylethylamine peak area (Y) and the concentration (X) are subjected to linear regression, and the result shows that the N, N-diisopropylethylamine and the N, N-diisopropylethylamine peak area have good linear relation in the concentration range of 12.5-37.5 mg/mL. Y=71398.8817x+4241.1206, r 2 ＝0.9979。
(2) Repeatability of
Six needles are continuously sampled from the working solution, and the repeatability of the method is inspected by using the peak area of N, N-diisopropylethylamine in the working solution. The RSD of the repeated measurement was 8.4%, which is satisfactory.
(3) Recovery rate of sample addition
3 samples of the same lot were weighed accurately and working solution (25. Mu.g/mL) was prepared as a solution having a concentration of praziquantel of about 25mg/mL, and the measurement results were shown in the following table.
Sample recovery rate results of N, N-diisopropylethylamine
(4) Detection limit
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather to be merely representative of the principles and spirit of the invention.
Claims (2)
1. A method for determining residual N, N-diisopropylethylamine in pleshafu by headspace gas chromatography, comprising the steps of:
(1) Taking a proper amount of pleshafu, dissolving the pleshafu with dimethyl sulfoxide (DMSO), and then fixing the volume with the dimethyl sulfoxide to prepare a sample solution with the concentration of the pleshafu of 25 mg/mL;
(2) Taking a proper amount of N, N-diisopropylethylamine, dissolving with dimethyl sulfoxide (DMSO), and then fixing the volume with the dimethyl sulfoxide to prepare a reference substance solution with the concentration of 0.025mg/mL of N, N-diisopropylethylamine;
(3) Taking N, N-diisopropylethylamine reference substance solution, and a pleshafu test substance solution, measuring residual N, N-diisopropylethylamine in pleshafu by adopting a headspace gas chromatography, adjusting detection sensitivity to ensure that the peak height of N, N-diisopropylethylamine in the reference substance solution is obvious, and if the peak area of the N, N-diisopropylethylamine position in the pleshafu test substance solution is not larger than the peak area of the peak position of the N, N-diisopropylethylamine working substance solution, adopting a quartz capillary column as a chromatographic column for measurement, adopting an inert gas as a gas source, adopting a temperature programming mode and a shunting mode by adopting the column, and a FID detector, wherein the inert gas can select nitrogen or helium, the length of the quartz capillary column is between 30m and 60m, the column diameter is between 0.25mm and 0.53mm, and the coating thickness is between 0.25 mu m and 3 mu m, and when the carrier gas source is nitrogen, the temperature programming condition is: the initial temperature is 40-60 ℃, the heating rate is 10-30 ℃/min, the final temperature is 200-280 ℃, the maintaining time is 1-10 min, the split ratio is 5:1, and the linear speed is 15-50 cm/s; the headspace temperature is 80-150 ℃, the shaking time is 15-60 minutes, and the sample inlet temperature is 180-250 ℃; taking 1mL of the FID detector, the temperature of the detector is 260 ℃, and the N, N-diisopropylethylamine reference substance solution and the pleshafu sample solution are respectively put into a headspace bottle, pressing a cover, putting into a headspace sample injector, setting the headspace temperature to be 80-150 ℃ and the shaking time to be 15-60 minutes, and injecting samples according to the method.
2. The method of claim 1, wherein the quartz capillary chromatography column has a length of 30m, a column diameter of 0.32mm, and a coating thickness of 3 μm; the temperature programming is as follows: the initial temperature is 40 ℃, the heating rate is 15 ℃/min, the final temperature is 240 ℃, and the temperature is maintained for 2min.
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| WO2014125499A1 (en) * | 2013-02-13 | 2014-08-21 | Natco Pharma Limited | Improved and commercially viable process for the preparation of high pure plerixafor base |
| CN110123742A (en) * | 2019-03-29 | 2019-08-16 | 四川汇宇制药有限公司 | A kind of preparation method of high-quality Plerixafor injection |
| CN110320293A (en) * | 2019-06-28 | 2019-10-11 | 北京澳合药物研究院有限公司 | A kind of method of residual solvent in measurement phthalide analog compound |
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Patent Citations (3)
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|---|---|---|---|---|
| WO2014125499A1 (en) * | 2013-02-13 | 2014-08-21 | Natco Pharma Limited | Improved and commercially viable process for the preparation of high pure plerixafor base |
| CN110123742A (en) * | 2019-03-29 | 2019-08-16 | 四川汇宇制药有限公司 | A kind of preparation method of high-quality Plerixafor injection |
| CN110320293A (en) * | 2019-06-28 | 2019-10-11 | 北京澳合药物研究院有限公司 | A kind of method of residual solvent in measurement phthalide analog compound |
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| Title |
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| synthesis and structural-activity relationships of azamacrocylic C-X-C chemokine receptor 4antagonists:analogues containing a single azamacrocyclic ring are potent inhibitiors of T-cell tropic(X4) HIV-1replication;Gary J. Bridger, Renato T. Skerlj;Journal of medicinal chemistry;第53卷;1250-1260 * |
| 一种强效造血干细胞动员剂——普乐沙福;杨华，朱知梅;中国现代药物应用;第16卷(第6期);249-252 * |
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