CN114295746A - Analysis and detection method of pitavastatin calcium - Google Patents
Analysis and detection method of pitavastatin calcium Download PDFInfo
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- CN114295746A CN114295746A CN202111616573.3A CN202111616573A CN114295746A CN 114295746 A CN114295746 A CN 114295746A CN 202111616573 A CN202111616573 A CN 202111616573A CN 114295746 A CN114295746 A CN 114295746A
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- 229960003296 pitavastatin calcium Drugs 0.000 title claims abstract description 50
- RHGYHLPFVJEAOC-FFNUKLMVSA-L pitavastatin calcium Chemical compound [Ca+2].[O-]C(=O)C[C@H](O)C[C@H](O)\C=C\C1=C(C2CC2)N=C2C=CC=CC2=C1C1=CC=C(F)C=C1.[O-]C(=O)C[C@H](O)C[C@H](O)\C=C\C1=C(C2CC2)N=C2C=CC=CC2=C1C1=CC=C(F)C=C1 RHGYHLPFVJEAOC-FFNUKLMVSA-L 0.000 title claims abstract description 50
- 238000001514 detection method Methods 0.000 title claims abstract description 15
- 238000004458 analytical method Methods 0.000 title claims abstract description 9
- 239000012085 test solution Substances 0.000 claims abstract description 19
- 239000012071 phase Substances 0.000 claims abstract description 17
- 239000012088 reference solution Substances 0.000 claims abstract description 15
- 239000012490 blank solution Substances 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 11
- 239000012074 organic phase Substances 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000010812 external standard method Methods 0.000 claims abstract description 7
- 238000010521 absorption reaction Methods 0.000 claims abstract description 6
- 238000004128 high performance liquid chromatography Methods 0.000 claims abstract description 4
- 238000002347 injection Methods 0.000 claims abstract description 4
- 239000007924 injection Substances 0.000 claims abstract description 4
- 238000010829 isocratic elution Methods 0.000 claims abstract description 4
- 238000004445 quantitative analysis Methods 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 26
- 239000012535 impurity Substances 0.000 claims description 26
- 239000000243 solution Substances 0.000 claims description 18
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical group CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 8
- 238000007865 diluting Methods 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 6
- 239000008346 aqueous phase Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- -1 2-cyclopropyl-4-phenylquinolin-3-yl Chemical group 0.000 claims description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 4
- 229960000583 acetic acid Drugs 0.000 claims description 2
- 239000012362 glacial acetic acid Substances 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 239000012445 acidic reagent Substances 0.000 claims 2
- 239000007788 liquid Substances 0.000 description 6
- 230000014759 maintenance of location Effects 0.000 description 6
- HVYWMOMLDIMFJA-DPAQBDIFSA-N cholesterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CCCC(C)C)[C@@]1(C)CC2 HVYWMOMLDIMFJA-DPAQBDIFSA-N 0.000 description 4
- 108010007622 LDL Lipoproteins Proteins 0.000 description 3
- 102000007330 LDL Lipoproteins Human genes 0.000 description 3
- 238000010828 elution Methods 0.000 description 3
- CABVTRNMFUVUDM-VRHQGPGLSA-N (3S)-3-hydroxy-3-methylglutaryl-CoA Chemical compound O[C@@H]1[C@H](OP(O)(O)=O)[C@@H](COP(O)(=O)OP(O)(=O)OCC(C)(C)[C@@H](O)C(=O)NCCC(=O)NCCSC(=O)C[C@@](O)(CC(O)=O)C)O[C@H]1N1C2=NC=NC(N)=C2N=C1 CABVTRNMFUVUDM-VRHQGPGLSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 235000012000 cholesterol Nutrition 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 229960002797 pitavastatin Drugs 0.000 description 2
- VGYFMXBACGZSIL-MCBHFWOFSA-N pitavastatin Chemical compound OC(=O)C[C@H](O)C[C@H](O)\C=C\C1=C(C2CC2)N=C2C=CC=CC2=C1C1=CC=C(F)C=C1 VGYFMXBACGZSIL-MCBHFWOFSA-N 0.000 description 2
- 239000013558 reference substance Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 108010028554 LDL Cholesterol Proteins 0.000 description 1
- 102000000853 LDL receptors Human genes 0.000 description 1
- 108010001831 LDL receptors Proteins 0.000 description 1
- 108090000854 Oxidoreductases Proteins 0.000 description 1
- 230000003042 antagnostic effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 210000005229 liver cell Anatomy 0.000 description 1
- 108020004999 messenger RNA Proteins 0.000 description 1
- 102000005962 receptors Human genes 0.000 description 1
- 108020003175 receptors Proteins 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- UFTFJSFQGQCHQW-UHFFFAOYSA-N triformin Chemical compound O=COCC(OC=O)COC=O UFTFJSFQGQCHQW-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention provides an analysis and detection method of pitavastatin calcium, which comprises the following steps: s1: preparing a blank solution, a reference solution and a test solution; s2, detecting the blank solution, the reference solution and the test solution by adopting a high performance liquid chromatography; the chromatographic conditions are as follows: the chromatographic column is an Agilent chromatographic column or a Phenomenex Luna PFP (2) chromatographic column, the temperature of the chromatographic column is 25 to 35 ℃, the flow rate is 0.8 to 1.2ml/min, the sample injection amount is 10 to 20 mu l, the detector is an ultraviolet absorption light detector, the mobile phase consists of a water phase and an organic phase, and isocratic elution is set according to volume fraction; and quantitative analysis is carried out by using an external standard method. The method for analyzing and detecting the pitavastatin calcium can accurately determine the content of the pitavastatin calcium and has good reproducibility.
Description
Technical Field
The invention relates to the technical field of drug analysis, in particular to an analysis and detection method of pitavastatin calcium.
Background
Pitavastatin has a strong antagonistic inhibition effect on hydroxymethylglutaryl coenzyme A (HMG-CoA) reductase, and can efficiently inhibit the process of generating cholesterol in human liver cells HepG2, thereby inhibiting the synthesis of cholesterol. Pitavastatin induces the synthesis of Low Density Lipoprotein (LDL) receptor mRNA at ultra low concentrations, increases its amount, causes an increase in LDL receptor density, promotes the clearance of LDL, and lowers plasma LDL-C concentration and plasma total triglyceride concentration.
When pitavastatin calcium is prepared by the existing method, impurities are generated, and the main impurities comprise an impurity A which is named as: (3r, 5s, e) -7- (2-cyclopropyl-4-phenylquinolin-3-yl) -3, 5-dihydroxy-6-enoic acid monocalcium having the structural formula:
Therefore, an effective method for analyzing and detecting pitavastatin calcium and impurity a is needed.
Disclosure of Invention
The invention aims to disclose an analysis and detection method of pitavastatin calcium, which can accurately determine the content of pitavastatin calcium and has good reproducibility.
In order to achieve the above object, the present invention provides an analytical detection method of pitavastatin calcium, comprising the steps of:
s1: preparing a blank solution, a reference solution and a test solution; the blank solution is ethanol, and the reference solution is prepared by dissolving pitavastatin calcium impurity A in ethanol and diluting to obtain a solution containing about 0.5 mu g/ml of pitavastatin calcium impurity A in each 1 ml; the test solution is prepared by dissolving pitavastatin calcium in ethanol and diluting to obtain a solution containing about 0.5mg/ml of pitavastatin calcium in each 1 ml; wherein, the pitavastatin calcium impurity A is named as: (3r, 5s, e) -7- (2-cyclopropyl-4-phenylquinolin-3-yl) -3, 5-dihydroxy-6-enoic acid monocalcium having the structural formula:
s2, detecting the blank solution, the reference solution and the test solution by adopting a high performance liquid chromatography; the chromatographic conditions are as follows: the chromatographic column is an Agilent chromatographic column or a Phenomenex Luna PFP (2) chromatographic column, the temperature of the chromatographic column is 25 to 35 ℃, the flow rate is 0.8 to 1.2ml/min, the sample injection amount is 10 to 20 mu l, the detector is an ultraviolet absorption light detector, the mobile phase consists of a water phase and an organic phase, and isocratic elution is set according to volume fraction; and quantitative analysis is carried out by using an external standard method.
Further, the aqueous phase comprises water and an acid agent which is phosphoric acid, glacial acetic acid or a mixture thereof.
Further, the pH of the aqueous phase in the mobile phase is between 3 and 5, said pH being adjusted by the acid agent.
Further, the solvent of the organic phase is selected from acetonitrile, ethanol, methanol or a mixture thereof.
Further, the volume ratio of the aqueous phase to the organic phase in the fluidity is 1: 1 to 7: 3.
further, the detection wavelength of the ultraviolet absorption light detector is 242nm to 246 nm. Within the wavelength range, the base line is stable, the peak type symmetry is good, and the reproducibility is good.
Compared with the prior art, the invention has the beneficial effects that: by the detection method disclosed by the invention, pitavastatin calcium can obtain a better peak type, and the elution time is more ideal. Within this range of flow rates, better peak theoretical plate counts and more optimal elution times are obtained.
Drawings
FIG. 1 is a chromatogram of an empty white solution in example 1 of the present invention;
FIG. 2 is a chromatogram of a test solution in example 1 of the present invention;
FIG. 3 is a chromatogram of a control solution in example 1 of the present invention;
FIG. 4 is a chromatogram of a test solution in example 2 of the present invention;
FIG. 5 is a chromatogram of a control solution in example 2 of the present invention.
Detailed Description
The present invention is described in detail below with reference to various embodiments, but it should be understood that these embodiments are not intended to limit the present invention, and those skilled in the art should be able to make modifications and substitutions on the functions, methods, or structures of these embodiments without departing from the scope of the present invention.
In the present application, the term "external standard method" refers to a method of quantifying the amount of a component to be measured in a sample by comparing the response signals of the component to be measured with those of the control substance using a pure product of the component to be measured as a control substance. The term "gradient elution" refers to the manner in which the composition of the mobile phase changes over time during the analysis cycle of the sample components.
The invention provides an analysis and detection method of pitavastatin calcium, which comprises the following steps:
s1: preparing a blank solution, a reference solution and a test solution; the blank solution is ethanol, and the reference solution is prepared by dissolving pitavastatin calcium impurity A in ethanol and diluting to obtain a solution containing about 0.5 mu g/ml of pitavastatin calcium impurity A in each 1 ml; the test solution is prepared by dissolving pitavastatin calcium in ethanol and diluting to obtain a solution containing about 0.5mg/ml of pitavastatin calcium in each 1 ml; wherein, the pitavastatin calcium impurity A is named as: (3r, 5s, e) -7- (2-cyclopropyl-4-phenylquinolin-3-yl) -3, 5-dihydroxy-6-enoic acid monocalcium having the structural formula:
s2, detecting the blank solution, the reference solution and the test solution by adopting a high performance liquid chromatography; the chromatographic conditions are as follows: the chromatographic column is an Agilent chromatographic column or a Phenomenex Luna PFP (2) chromatographic column, the temperature of the chromatographic column is 25 to 35 ℃, the flow rate is 0.8 to 1.2ml/min, the sample injection amount is 10 to 20 mu l, the detector is an ultraviolet absorption light detector, the mobile phase consists of a water phase and an organic phase, and isocratic elution is set according to volume fraction; and quantitative analysis is carried out by using an external standard method.
Example 1
Using an Agilent column, 150 x 4.6mm,5 mu or equivalent, adjusting the pH value of the water phase in the mobile phase to 4.0 by using phosphoric acid, and adjusting the volume ratio of the mobile phase to 70: 30 phosphate solution: acetonitrile, column temperature 30 ℃, detection wavelength 244nm, flow rate 1.0 ml/min.
Taking pitavastatin calcium, precisely weighing, adding ethanol for dissolving and diluting to prepare a solution containing about 0.5mg/ml of pitavastatin calcium in every 1 ml; preparing a reference substance solution of 0.5 mu g/ml pitavastatin calcium impurity A by the same method; and (3) taking 10 mu l of each of the reference solution and the test solution, injecting the reference solution and the test solution into a liquid chromatograph according to the chromatographic conditions, and recording a chromatogram. The content is calculated according to an external standard method.
As shown in FIG. 1, the spectrum of the blank solution is a horizontal straight line and no peak appears.
As shown in fig. 2, a high performance liquid chromatogram of the pitavastatin calcium test solution in example 1 is shown; in the figure, the retention time of the main peak of pitavastatin calcium is 12.8min, and the retention time of the impurity A is 2.534 min.
As shown in FIG. 3, which is a high performance liquid chromatogram of the pitavastatin calcium impurity A control solution in example 1, the retention time of the impurity A is 2.528 min.
Therefore, the method of example 1 can accurately detect the impurity a of pitavastatin calcium.
Example 2
Using Phenomenex Luna PFP (2) chromatographic column, 150 x 4.6mm,5 mu or equivalent chromatographic column, adjusting pH value of water phase in mobile phase to 4.5 by phosphoric acid, and adjusting volume ratio of mobile phase to 60: 40 phosphate solution: methanol at 30 deg.C, detection wavelength of 244nm, and flow rate of 0.8 ml/min.
Taking a proper amount of pitavastatin calcium, precisely weighing, adding a diluent to dissolve and dilute the pitavastatin calcium to prepare a solution containing about 0.5mg/ml of pitavastatin calcium in every 1ml of solution as a test solution; preparing a reference substance solution of 0.5 mu g/ml pitavastatin calcium impurity A by the same method; and (3) taking 10 mu l of each of the reference solution and the test solution, injecting the reference solution and the test solution into a liquid chromatograph according to the chromatographic conditions, and recording a chromatogram. And calculating the impurity content according to an external standard method.
As shown in fig. 4, is a high performance liquid chromatogram of the pitavastatin calcium test sample in example 2; in the figure, the retention time of the main peak of pitavastatin calcium is 12.9min, and the retention time of the impurity A is 2.530 min.
As shown in fig. 5, which is a high performance liquid chromatogram of the pitavastatin calcium impurity a control solution in example 2, the retention time of the impurity a in the figure is 2.534 min.
Therefore, the method of example 2 can also accurately detect the impurity a of pitavastatin calcium.
In the above two examples, the impurity a may be selected as it is from commercially available products of the family of mology north of Hu.
The above-listed detailed description is only a specific description of a possible embodiment of the present invention, and they are not intended to limit the scope of the present invention, and equivalent embodiments or modifications made without departing from the technical spirit of the present invention should be included in the scope of the present invention.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (6)
1. An analytical detection method of pitavastatin calcium is characterized by comprising the following steps:
s1: preparing a blank solution, a reference solution and a test solution; the blank solution is ethanol, and the reference solution is prepared by dissolving pitavastatin calcium impurity A in ethanol and diluting to obtain a solution containing about 0.5 mu g/ml of pitavastatin calcium impurity A in each 1 ml; the test solution is prepared by dissolving pitavastatin calcium in ethanol and diluting to obtain a solution containing about 0.5mg/ml of pitavastatin calcium in each 1 ml; wherein, the pitavastatin calcium impurity A is named as: (3r, 5s, e) -7- (2-cyclopropyl-4-phenylquinolin-3-yl) -3, 5-dihydroxy-6-enoic acid monocalcium having the structural formula:
s2, detecting the blank solution, the reference solution and the test solution by adopting a high performance liquid chromatography; the chromatographic conditions are as follows: the chromatographic column is an Agilent chromatographic column or a Phenomenex Luna PFP (2) chromatographic column, the temperature of the chromatographic column is 25 to 35 ℃, the flow rate is 0.8 to 1.2ml/min, the sample injection amount is 10 to 20 mu l, the detector is an ultraviolet absorption light detector, the mobile phase consists of a water phase and an organic phase, and isocratic elution is set according to volume fraction; and quantitative analysis is carried out by using an external standard method.
2. The analytical method for detecting pitavastatin calcium according to claim 1, characterized in that the aqueous phase comprises water and an acid reagent which is phosphoric acid, glacial acetic acid or a mixture thereof.
3. The analytical detection method of pitavastatin calcium according to claim 2, characterized in that the pH value of the aqueous phase in the mobile phase is 3 to 5, and the pH value is adjusted by an acid reagent.
4. The analytical detection method of pitavastatin calcium according to claim 3, characterized in that the solvent of the organic phase is selected from acetonitrile, ethanol, methanol or a mixture thereof.
5. The analytical detection method of pitavastatin calcium according to claim 4, characterized in that the volume ratio of the aqueous phase to the organic phase in the fluidity is 1: 1 to 7: 3.
6. the method for analyzing and detecting pitavastatin calcium as claimed in claim 5, wherein the ultraviolet absorption light detector detects the wavelength of 242nm to 246 nm.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115389655A (en) * | 2022-08-11 | 2022-11-25 | 唯智医药科技（北京）有限公司 | 6-formaldehyde-2,2 dimethyl-1,3-dioxane-4-tert-butyl acetate isomer impurity detection |
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2021
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115389655A (en) * | 2022-08-11 | 2022-11-25 | 唯智医药科技（北京）有限公司 | 6-formaldehyde-2,2 dimethyl-1,3-dioxane-4-tert-butyl acetate isomer impurity detection |
| CN115389655B (en) * | 2022-08-11 | 2024-04-09 | 唯智医药科技（北京）有限公司 | Detection of impurity of 6-formoxyl-2, 2 dimethyl-1, 3-dioxane-4-tert-butyl acetate isomer |
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