CN113484445A - Method for detecting content of 5-chloropentanoic acid - Google Patents
Method for detecting content of 5-chloropentanoic acid Download PDFInfo
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- CN113484445A CN113484445A CN202110885556.3A CN202110885556A CN113484445A CN 113484445 A CN113484445 A CN 113484445A CN 202110885556 A CN202110885556 A CN 202110885556A CN 113484445 A CN113484445 A CN 113484445A
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- YSXDKDWNIPOSMF-UHFFFAOYSA-N 5-chloropentanoic acid Chemical compound OC(=O)CCCCCl YSXDKDWNIPOSMF-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 24
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000003085 diluting agent Substances 0.000 claims abstract description 21
- 239000003814 drug Substances 0.000 claims abstract description 16
- 238000001514 detection method Methods 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000001819 mass spectrum Methods 0.000 claims abstract description 9
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000005695 Ammonium acetate Substances 0.000 claims abstract description 8
- 229940043376 ammonium acetate Drugs 0.000 claims abstract description 8
- 235000019257 ammonium acetate Nutrition 0.000 claims abstract description 8
- 238000010828 elution Methods 0.000 claims abstract description 7
- 238000007865 diluting Methods 0.000 claims abstract description 6
- 239000000945 filler Substances 0.000 claims abstract description 6
- 238000004458 analytical method Methods 0.000 claims abstract description 5
- 239000007864 aqueous solution Substances 0.000 claims abstract description 5
- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 4
- 239000012085 test solution Substances 0.000 claims abstract description 4
- 238000004811 liquid chromatography Methods 0.000 claims abstract description 3
- 239000012088 reference solution Substances 0.000 claims abstract description 3
- 239000002904 solvent Substances 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 6
- 238000013467 fragmentation Methods 0.000 claims description 3
- 238000006062 fragmentation reaction Methods 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 238000004949 mass spectrometry Methods 0.000 claims description 2
- 238000002552 multiple reaction monitoring Methods 0.000 claims 1
- 229940079593 drug Drugs 0.000 abstract description 12
- 230000035945 sensitivity Effects 0.000 abstract description 4
- 239000007788 liquid Substances 0.000 abstract description 3
- 239000011550 stock solution Substances 0.000 description 28
- 239000013558 reference substance Substances 0.000 description 12
- 238000005303 weighing Methods 0.000 description 8
- 239000000523 sample Substances 0.000 description 6
- 239000012488 sample solution Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000000889 atomisation Methods 0.000 description 2
- 239000012490 blank solution Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000000132 electrospray ionisation Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 238000012417 linear regression Methods 0.000 description 1
- 230000007721 medicinal effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
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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
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
- G01N30/7233—Mass spectrometers interfaced to liquid or supercritical fluid chromatograph
-
- 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
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
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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)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention relates to a method for detecting the content of 5-chloropentanoic acid, which comprises the following steps: taking a diluent as a solvent for raw material medicines to prepare a test solution, taking 5-chloropentanoic acid, dissolving with methanol, and diluting with the diluent to prepare a reference solution; step two, performing liquid chromatography analysis by using octadecylsilane chemically bonded silica as a filler, and performing gradient elution by using an ammonium acetate aqueous solution as a mobile phase A and methanol as a mobile phase B; and step three, performing mass spectrum detection by adopting a mass spectrum detector. The method for detecting the content of 5-chlorovaleric acid provided by the invention uses a high performance liquid chromatography-mass spectrometer for detection, has the advantages of high sensitivity, good accuracy, good repeatability and the like, and can be widely used for detecting the content of 5-chlorovaleric acid in raw material medicines.
Description
Technical Field
The embodiment of the invention belongs to the technical field of analysis and detection of raw material medicines, and particularly relates to a method for detecting the content of 5-chlorovaleric acid.
Background
The raw material medicaments for producing various preparations have important value in the pharmaceutical industry. The purity and impurity content of the raw material medicaments have important influence on the medical effect and safety of the medicinal preparation. The production process of the bulk drug has the characteristics of itself, and often comprises complex chemical change and biological change processes, and byproducts or redundant raw material residues are generated.
At present, some raw material medicines are mixed with certain content of 5-chloropentanoic acid in the production process, the 5-chloropentanoic acid has certain toxicity and irritation, and in order to ensure the final purity and safety of the raw material medicines, the analysis and control of the content of the 5-chloropentanoic acid in the raw material medicines are of great significance.
Therefore, it is necessary to develop a new method for detecting and analyzing the content of 5-chloropentanoic acid in a bulk drug.
Disclosure of Invention
After the intensive research, the inventor provides a method for detecting the content of 5-chloropentanoic acid, and the method has the advantages of high sensitivity, good accuracy, good repeatability and the like.
A method for detecting the content of 5-chloropentanoic acid comprises the following steps:
taking a diluent as a solvent for raw material medicines to prepare a test solution, taking 5-chloropentanoic acid, dissolving with methanol, and diluting with the diluent to prepare a reference solution;
step two, performing liquid chromatography analysis by using octadecylsilane chemically bonded silica as a filler, and performing gradient elution by using an ammonium acetate aqueous solution as a mobile phase A and methanol as a mobile phase B;
and step three, performing mass spectrum detection by adopting a mass spectrum detector.
Preferably, in step one, the control solution contains 15ng to 300ng of 5-chloropentanoic acid per 1mL, and more preferably, the control solution contains 150ng of 5-chloropentanoic acid per 1 mL.
Preferably, in the second step, the filler has an inner diameter of 2.1mm, a column length of 50mm and a particle diameter of 1.8. mu.m.
Preferably, in the second step, the concentration of the ammonium acetate aqueous solution is 10 mmol/L.
Preferably, in step two, the column temperature is 40 ℃, the flow rate is 0.3mL per minute, and the sample volume is 10. mu.L.
Preferably, in the second step, the specific process of gradient elution is as follows:
the time is 0.00 minute, the volume ratio of the mobile phase A is 90 percent, and the volume ratio of the mobile phase B is 10 percent;
the time is 1.00 minute, the volume ratio of the mobile phase A is 90 percent, and the volume ratio of the mobile phase B is 10 percent;
the time is 1.20 minutes, the volume ratio of the mobile phase A is 5 percent, and the volume ratio of the mobile phase B is 95 percent;
the time is 4.00 minutes, the volume ratio of the mobile phase A is 5 percent, and the volume ratio of the mobile phase B is 95 percent;
the time is 4.20 minutes, the volume ratio of the mobile phase A is 90 percent, and the volume ratio of the mobile phase B is 10 percent;
the time is 6.00 minutes, the volume ratio of the mobile phase A is 90 percent, and the volume ratio of the mobile phase B is 10 percent.
Preferably, in the third step, the mass spectrometry detection adopts an electrospray ionization source (ESI) and a negative ion detection mode, the capillary voltage is 2000V, the sheath gas temperature is 250 ℃, the drying gas temperature is 320 ℃, the drying gas flow rate is 4L/min, and the atomization gas is 40 psi.
Preferably, in the third step, in a multi-reaction monitoring scanning mode, ion pairs m/z135.02-35.2 are collected as qualitative and quantitative ion pairs, the collision energy is 5eV, the fragmentation voltage is 62V, and the scanning time is 200 msec.
Compared with the prior art, the invention has the following beneficial effects:
the method for detecting the content of 5-chloropentanoic acid in the bulk drugs provided by the invention uses a high performance liquid chromatography-mass spectrometer for detection, has the advantages of high sensitivity, good accuracy, good repeatability and the like, and can be widely used for detecting the content of 5-chloropentanoic acid in the bulk drugs.
Drawings
FIG. 1 is a linear regression graph of an embodiment of the present invention.
FIG. 2 is a typical diagram of a blank solution according to an embodiment of the present invention.
FIG. 3 is a typical view of a control solution according to an embodiment of the present invention.
FIG. 4 is a typical view of a sample solution according to an embodiment of the present invention.
Detailed Description
A method for detecting the content of 5-chloropentanoic acid in bulk drugs comprises the following steps:
solution preparation:
diluent agent: precisely weighing about 770.83mg of ammonium acetate, placing the ammonium acetate in 1000mL of ultrapure water, and shaking up; putting 450mL of the solution into a mobile phase bottle, adding 50mL of methanol, shaking up the solution to be used as a blank solution;
5-Chloropentanoic acid control stock solution: taking about 20mg of a 5-chloropentanoic acid reference substance, accurately weighing, placing in a 20mL measuring flask, adding methanol for dissolving and diluting to scale, shaking up, accurately weighing 1mL, placing in a 20mL measuring flask, adding methanol for diluting to scale, shaking up, accurately weighing 1.5mL, placing in a 50mL measuring flask, adding a diluent for diluting to scale, and shaking up to obtain (1500 ng/mL);
control Solution (STD): precisely measuring 1mL of 5-chloropentanoic acid reference substance stock solution, placing the stock solution in a 10mL measuring flask, adding a diluent to dilute the stock solution to a scale, and shaking up to obtain (150 ng/mL);
200% linear solution: precisely measuring 4mL of 5-chloropentanoic acid reference substance stock solution, placing the stock solution in a 20mL measuring flask, adding a diluent to dilute the stock solution to a scale, and shaking up;
150% linear solution: precisely measuring 3mL of a 5-chloropentanoic acid reference substance stock solution, placing the stock solution in a 20mL measuring flask, adding a diluent to dilute the stock solution to a scale, and shaking up;
100% linear solution: precisely measuring 2mL of a 5-chloropentanoic acid reference substance stock solution, placing the stock solution in a 20mL measuring flask, adding a diluent to dilute the stock solution to a scale, and shaking up;
75% linear solution: precisely measuring 1.5mL of a 5-chloropentanoic acid reference substance stock solution, placing the stock solution in a 20mL measuring flask, adding a diluent to dilute the stock solution to a scale, and shaking up;
50% linear solution: precisely measuring 1mL of 5-chloropentanoic acid reference substance stock solution, placing the stock solution in a 20mL measuring flask, adding a diluent to dilute the stock solution to a scale, and shaking up;
25% linear solution: precisely measuring 0.5mL of 5-chloropentanoic acid reference substance stock solution, placing the stock solution in a 20mL measuring flask, adding a diluent to dilute the stock solution to a scale, and shaking up;
LOQ: precisely measuring 0.5mL of 5-chloropentanoic acid reference substance stock solution, placing the stock solution in a 20mL measuring flask, adding a diluent to dilute the stock solution to a scale, shaking up, and preparing 6 parts in parallel;
LOD: precisely measuring 1mL of a 100% linear solution of 5-chloropentanoic acid, placing the linear solution in a 10mL measuring flask, adding a diluent to dilute the solution to a scale, and shaking up;
test solution: taking about 40mg of a test sample raw material medicine, accurately weighing, placing in a 20mL measuring flask, adding a diluent to dissolve and dilute to a scale, shaking up, and preparing 3 parts in parallel;
50% of the standard sample solution: taking about 40mg of a test sample, precisely weighing, placing in a 20mL measuring flask, precisely measuring into 1mL of a reference substance stock solution, adding a diluent to dissolve and dilute to a scale, shaking up, and preparing 3 parts in parallel;
100% of the standard sample solution: taking about 40mg of a test sample, precisely weighing, placing in a 20mL measuring flask, precisely measuring 2mL of a reference substance stock solution, adding a diluent to dissolve and dilute to a scale, shaking up, and parallelly preparing 6 parts;
150% of the standard sample solution: taking about 40mg of a test sample, precisely weighing, placing in a 20mL measuring flask, precisely measuring 3mL of a reference substance stock solution, adding a diluent to dissolve and dilute to a scale, shaking up, and preparing 3 parts in parallel;
the test method comprises the following steps:
performing high performance liquid chromatography with octadecylsilane chemically bonded silica as filler (Agilen Agilent ZORBAX Eclipse plus chromatographic column inner diameter of 2.1mm, column length of 50mm, and particle diameter of 1.8 μm); taking 10mmol/L ammonium acetate aqueous solution as a mobile phase A and methanol as a mobile phase B, and carrying out gradient elution according to the table 1; the column temperature was 40 ℃; the flow rate is 0.3mL per minute; the sample volume is 10 mu L;
and finally, performing mass spectrum detection by using a mass spectrum detector, wherein the mass spectrum detector adopts an electrospray ionization source (ESI) and a negative ion detection mode, the capillary voltage is 2000V, the sheath gas temperature is 250 ℃, the drying gas temperature is 320 ℃, the drying gas flow rate is 4L/min, the atomization gas is 40psi, a multi-reaction monitoring scanning mode is adopted, an ion pair m/z135.02-35.2 is collected as a qualitative and quantitative ion pair, the collision energy is 5eV, the fragmentation voltage is 62V, and the scanning time is 200 msec.
TABLE 1 gradient elution Table
| Time (minutes) | Mobile phase A (%) | Mobile phase B (%) |
| 0.00 | 90 | 10 |
| 1.00 | 90 | 10 |
| 1.20 | 5 | 95 |
| 4.00 | 5 | 95 |
| 4.20 | 90 | 10 |
| 6.00 | 90 | 10 |
TABLE 2 Linear results
TABLE 3 quantitation Limit and detection Limit results
TABLE 4 quantitative limit results
TABLE 5 accuracy results
TABLE 6 repeatability results
TABLE 7 stability results
With reference to tables 1 to 7 and fig. 1 to 4, the method for detecting the content of 5-chlorovaleric acid in bulk pharmaceutical chemicals provided by this embodiment uses a high performance liquid chromatography-mass spectrometer for detection, has the advantages of high sensitivity, good accuracy, good repeatability and the like, and can be widely used for detecting the content of 5-chlorovaleric acid in bulk pharmaceutical chemicals.
Claims (9)
1. A method for detecting the content of 5-chloropentanoic acid is characterized by comprising the following steps:
taking a raw material medicament and a diluent as a solvent to prepare a test solution, taking 5-chloropentanoic acid, dissolving the 5-chloropentanoic acid by using methanol, and diluting the solution by using the diluent to prepare a reference solution;
step two, performing liquid chromatography analysis by using octadecylsilane chemically bonded silica as a filler, and performing gradient elution by using an ammonium acetate aqueous solution as a mobile phase A and methanol as a mobile phase B;
and step three, performing mass spectrum detection by adopting a mass spectrum detector.
2. The method of claim 1, wherein in step one, the control solution contains 15ng to 300ng of 5-chloropentanoic acid per 1 mL.
3. The method of claim 2, wherein the control solution contains 150ng of 5-chloropentanoic acid per 1 mL.
4. The method of claim 1, wherein in step two, the filler has a size of 2.1mm in inner diameter, 50mm in column length, and 1.8 μm in particle size.
5. The method of claim 1, wherein in step two, the concentration of the aqueous ammonium acetate solution is 10 mmol/L.
6. The method of claim 1, wherein in step two, the column temperature is 40 ℃, the flow rate is 0.3mL per minute, and the sample size is 10 μ L.
7. The method of claim 1, wherein in the second step, the gradient elution is performed by the following specific process:
the time is 0.00 minute, the volume ratio of the mobile phase A is 90 percent, and the volume ratio of the mobile phase B is 10 percent;
the time is 1.00 minute, the volume ratio of the mobile phase A is 90 percent, and the volume ratio of the mobile phase B is 10 percent;
the time is 1.20 minutes, the volume ratio of the mobile phase A is 5 percent, and the volume ratio of the mobile phase B is 95 percent;
the time is 4.00 minutes, the volume ratio of the mobile phase A is 5 percent, and the volume ratio of the mobile phase B is 95 percent;
the time is 4.20 minutes, the volume ratio of the mobile phase A is 90 percent, and the volume ratio of the mobile phase B is 10 percent;
the time is 6.00 minutes, the volume ratio of the mobile phase A is 90 percent, and the volume ratio of the mobile phase B is 10 percent.
8. The method of claim 1, wherein in step three, the mass spectrometry detection is performed in electrospray ion source and negative ion detection mode, the capillary voltage is 2000V, the sheath gas temperature is 250 ℃, the drying gas temperature is 320 ℃, the drying gas flow rate is 4L/min, and the atomizing gas is 40 psi.
9. The method of claim 1, wherein in step three, ion pairs m/z135.02-35.2 are collected as qualitative and quantitative ion pairs in a multiple reaction monitoring scan mode, with a collision energy of 5eV, a fragmentation voltage of 62V, and a scan time of 200 msec.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116930370A (en) * | 2023-07-28 | 2023-10-24 | 辽源市百康药业有限责任公司 | Method for measuring parachloroaniline in paracetamol |
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2021
- 2021-08-03 CN CN202110885556.3A patent/CN113484445A/en active Pending
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