CN114062542A - Separation and detection method of lansoprazole nitrogen oxide impurities - Google Patents
Separation and detection method of lansoprazole nitrogen oxide impurities Download PDFInfo
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Abstract
The application relates to the field of pharmaceutical analysis, and particularly discloses a method for separating and detecting lansoprazole nitrogen oxide impurities. The method for separating and detecting the lansoprazole nitrogen oxide impurities uses octadecylsilane chemically bonded silica as a stationary phase, and adopts reversed-phase high performance liquid chromatography to detect a control sample, wherein the sum of the volume ratio of a mobile phase A and a mobile phase B is 100%, the polarity of the mobile phase is greater than that of the stationary phase, the mobile phase A is methanol, and the volume ratio of the mobile phase B is 100: (440-550): (4.4-6.0): and (0.9-2) eluting the solution with methanol-water-triethylamine-phosphoric acid according to a specific elution ratio. The method has the advantages that the peak-emerging time is moderate, the retention time difference between the impurity A and the nitrogen oxide impurity is large, the real main peak can be reflected, the accurate purity of the lansoprazole can be obtained, the technical gap of the detection of the lansoprazole nitrogen oxide impurity is filled, and the method has profound significance for the quality control of the lansoprazole.
Description
Technical Field
The application relates to the field of drug analysis, in particular to a method for separating and detecting lansoprazole nitrogen oxide impurities.
Background
Lansoprazole impurity A (C)16H14F3N3O3S) is an antacid drug with a structural formula
Is a proton pump inhibitor, is one of the most effective medicaments for inhibiting gastric acid secretion, is a medicament for assisting diseases such as peptic ulcer, reflux esophagitis and the like, and is used as an antacid medicament to be combined with other medicaments for treatment. The indications are gastric ulcer, duodenal ulcer and reflux esophagitis, and lansoprazole impurity A is mainly sold in the form of tablets around the world and is an effective drug with good tolerance.
Lansoprazole impurity A can generate different impurities in the production process, wherein one of the impurities is lansoprazole impurity A (C)16H14F3N3O3S) structural formula is
The other is the impurity (C) of lansoprazole nitrogen oxide impurity16H14F3N3O4S) structural formula is
After a compound enters Chinese pharmacopoeia, a general HPLC (high performance liquid chromatography) method is adopted to detect the compound, all impurities of lansoprazole are detected by the method, and the general method is generally applicable to all impurities of lansoprazole. However, since the structural formula of the lansoprazole nitrogen oxide impurity is different from that of the lansoprazole impurity A only by one sulfone, the structural electron cloudThe distribution situation can show that the polarities of the lansoprazole impurity A and the lansoprazole nitrogen oxide impurity are very close, peak signals of the lansoprazole impurity A and the lansoprazole nitrogen oxide impurity are difficult to distinguish through a chromatogram obtained by a pharmacopoeia detection method, so that the real main peak purity cannot be reflected, and the accurate purity of the lansoprazole cannot be obtained.
Therefore, in view of the above-mentioned related art, the inventors believe that the pharmacopoeia standard method cannot effectively separate and detect nitrogen oxide impurities generated from lansoprazole impurity a. Therefore, a method for accurately detecting the lansoprazole nitrogen oxide impurities needs to be developed, the technical gap of detecting the lansoprazole nitrogen oxide impurities is filled, and the method has profound significance for controlling the quality of the lansoprazole raw materials and the preparation thereof.
Disclosure of Invention
In order to improve the specificity of detecting the lansoprazole series impurities, the application provides a method for separating and detecting the lansoprazole nitrogen oxide impurities.
The application provides a separation method of lansoprazole nitrogen oxide impurities, which adopts the following technical scheme:
a separation method of lansoprazole nitrogen oxide impurities is characterized in that octadecylsilane chemically bonded silica is used as a stationary phase, a mobile phase A and a mobile phase B are used as mobile phases, a reversed-phase high performance liquid chromatography is adopted to detect a control sample, the sum of the volume ratio of the mobile phase A to the mobile phase B is 100%, the polarity of the mobile phase A is greater than that of the stationary phase, the mobile phase A is methanol, and the volume ratio of the mobile phase B is 100: (440-550): (4.4-6.0): (0.9-2) carrying out elution detection on the methanol-water-triethylamine-phosphoric acid solution according to the following elution gradient:
the initial volume ratio of the mobile phase A is 30-45%, the volume ratio of the mobile phase B is 55-70%, the mobile phase A is gradually adjusted to be 45-55% in 20min, the volume ratio of the mobile phase B is 45-55%, the volume ratio of the mobile phase A is adjusted to be 55-65% in 40min, and the volume ratio of the mobile phase B is 35-45%.
Due to the elution by adopting the elution gradient, each peak in the lansoprazole impurity A can achieve baseline separation, the retention time difference between the lansoprazole nitrogen oxide impurity and the lansoprazole impurity A is larger on the premise of moderate peak-out time, peak signals of the lansoprazole nitrogen oxide impurity A and the lansoprazole nitrogen oxide impurity can be obviously distinguished on a spectrogram, the separation degree of the lansoprazole nitrogen oxide impurity and the lansoprazole impurity A is increased by the elution gradient, a main peak can be truly reflected, the effective separation detection of the impurity A and the nitrogen oxide impurity is realized, and the accurate purity of the lansoprazole is obtained.
The detection method for separating and detecting the purity of the lansoprazole fills up the technical gap of separating and detecting the nitrogen oxide impurities of the lansoprazole, and has profound significance for controlling the quality of lansoprazole raw materials and preparations thereof.
Preferably, the elution gradient is:
preferably, the elution gradient is:
| time/min | Mobile phase A/%) | Mobile phase B/%) |
| 0 | 35 | 65 |
| 20 | 45 | 55 |
| 40 | 55 | 45 |
。
Through the elution gradient, the retention time of the lansoprazole impurity A and the lansoprazole nitrogen oxide impurity can be further prolonged, so that the separation degree between the two impurities is further increased, a real main peak can be reflected, the effective separation and detection of the impurity A and the nitrogen oxide impurity can be realized, and the accurate purity of the lansoprazole can be obtained.
Preferably, the pH value of the mobile phase B is 7.1-7.5.
Because the pH value of the mobile phase can influence the existing state of lansoprazole impurity impurities in the mobile phase, the adsorption and desorption effects between chromatographic columns can be influenced, and the retention time and separation can be influenced, the pH value of 7.1-7.5 is selected for the mobile phase B, so that the adsorption and desorption effects of the chromatographic columns are not easily influenced by the mobile phase, the existing state of the lansoprazole impurity in the mobile phase is not easily influenced, the separation degree of the two impurities is not easily influenced, and more accurate lansoprazole purity is obtained.
Preferably, the volume ratio of methanol-water-triethylamine-phosphoric acid is 100: (500-550): (5.0-6.0): (1.5-2.0).
Preferably, the methanol-water-triethylamine-phosphoric acid is prepared from a mixture of methanol-water-triethylamine-phosphoric acid and methanol-water-triethylamine-phosphoric acid in a volume ratio of 100: 440: 4.4: 0.9.
because the mobile phase B is prepared by methanol-water-triethylamine-phosphoric acid in a specific way, and forms an integral high performance liquid chromatography detection system with the mobile phase A and the silane column, the lansoprazole nitrogen oxide impurities and the lansoprazole impurities A are better distinguished by utilizing the selection of polarity, and thus the more accurate purity of the lansoprazole is obtained.
The application provides a method for detecting lansoprazole nitrogen oxide impurities, which adopts the following technical scheme:
and (3) putting the sample solution into a high performance liquid chromatography tester, wherein the sample injection volume is 5ul during testing.
By adopting the technical scheme, the elution gradient and the selection of octadecylsilane chemically bonded silica are matched, and 5ul of sample injection amount is adopted, so that the fluidity is not easy to exceed a linear range due to impact caused by overlarge sample injection amount, the retention capacity of a stationary phase is not easy to be interfered, and simultaneously, the test result is not accurate due to too low sample injection amount and too large influence of noise; therefore, the separation degree of the lansoprazole impurity A and the lansoprazole nitrogen oxide impurity is further improved by selecting a proper sample amount, so that the purity of the medicine can be more accurately reflected.
Preferably, the column temperature is 32-38 ℃ during the test.
More preferably, the column temperature is 35 ℃ when measured.
By adopting the technical scheme, the column temperature is set to be 32-38 ℃, so that the peak shapes of two impurities difficult to separate are better, the detection and analysis time is shortened, and the impurity separation efficiency is improved.
Preferably, the detection wavelength is 284nm, and the operation is carried out in a dark place.
In summary, the present application has the following beneficial effects:
1. because the elution is carried out by adopting the set elution gradient, the retention time difference between the lansoprazole nitrogen oxide impurities and the lansoprazole impurities A is larger, the separation degree between the lansoprazole nitrogen oxide impurities and the lansoprazole impurities A is increased, the impurities A and the nitrogen oxide impurities are effectively separated and detected, the technical gap of lansoprazole nitrogen oxide impurity detection is filled, and the method has profound significance for the quality control of the lansoprazole raw materials and the preparation thereof.
2. In the application, the mobile phase B is preferably prepared from methanol-water-triethylamine-phosphoric acid in a specific manner, and forms an integral high performance liquid chromatography detection system with the mobile phase A and a silane column, and the lansoprazole nitrogen oxide impurities and the lansoprazole impurities A are better distinguished by utilizing the selection of polarity, so that more accurate purity of the lansoprazole is obtained.
3. This application adopts 5 ul's sample size, further improves the separation degree of surveying lansoprazole impurity A and lansoprazole nitrogen oxide impurity to can reflect the purity of medicine more accurately.
Drawings
FIGS. 1-16 are HPLC charts of examples 1-15 of the present application and comparative example 1, respectively.
Detailed Description
The present application will be described in further detail with reference to the following drawings and examples.
Examples
Example 1
The embodiment discloses a method for separating and detecting lansoprazole nitrogen oxide impurities.
Taking about 10mg of lansoprazole impurity mixed sample (sold in the market) and about 10mg of m-chloroperoxybenzoic acid, putting the lansoprazole impurity mixed sample and the m-chloroperoxybenzoic acid into the same 20ml measuring flask, adding a methanol-water (60: 40) solution to dissolve and dilute the mixture to a scale, standing the mixture for 10 minutes, taking 10 mu l of a chromatographic column (specification: 4.6mm multiplied by 250mm and 5 mu m) filled with octadecylsilane bonded silica gel as a filler, taking methanol as a mobile phase A, taking a methanol-water-triethylamine-phosphoric acid solution with a volume ratio (100: 440: 4.4: 0.9) as a mobile phase B, adjusting the pH value to 7.1 by using a phosphoric acid solution (1 → 10), wherein the detection wavelength is 284nm, the sample injection volume is 5 mu l, the column temperature is 35 ℃, and carrying out elution detection according to the elution gradient shown in the table 1.
TABLE 1
The HPLC profile was observed, see FIG. 1: the retention time of the lansoprazole impurity A is 10.356min, and the retention time of the lansoprazole nitrogen oxide impurity is 11.787 min.
Example 2
The embodiment discloses a method for separating and detecting lansoprazole nitrogen oxide impurities.
The difference from example 1 is that the elution gradient is shown in Table 2.
TABLE 2
Observe the HPLC profile, see fig. 2: the retention time of the lansoprazole impurity A is 5.min, and the retention time of the lansoprazole nitrogen oxide impurity is 6.231 min.
Example 3
The embodiment discloses a method for separating and detecting lansoprazole nitrogen oxide impurities.
The difference from example 1 is that the elution gradient is shown in Table 3.
TABLE 3
Observe the HPLC profile, see fig. 3: the retention time of the lansoprazole impurity A is 9.138min, and the retention time of the lansoprazole nitrogen oxide impurity is 10.400 min.
Example 4
The embodiment discloses a method for separating and detecting lansoprazole nitrogen oxide impurities.
The difference from example 1 is that the elution gradient is shown in Table 4.
TABLE 4
The HPLC profile was observed, see FIG. 4: the retention time of the lansoprazole impurity A is 8.801min, and the retention time of the lansoprazole nitrogen oxide impurity is 10.518 min.
Example 5
The embodiment discloses a method for separating and detecting lansoprazole nitrogen oxide impurities.
The difference from example 1 is that the elution gradient is shown in Table 5.
TABLE 5
The HPLC profile was observed, see FIG. 5: the retention time of the lansoprazole impurity A is 5.508min, and the retention time of the lansoprazole nitrogen oxide impurity is 6.310 min.
Example 6
The embodiment discloses a method for separating and detecting lansoprazole nitrogen oxide impurities.
The difference from example 5 is that: the injection volume was 10 ul.
Observe the HPLC profile, see fig. 6: the peaks of lansoprazole impurity a and lansoprazole nitrogen oxide impurity are not completely separated.
Example 7
The embodiment discloses a method for separating and detecting lansoprazole nitrogen oxide impurities.
The difference from example 5 is that: the injection volume was 15 ul.
The HPLC profile was observed, see FIG. 7: the peaks of lansoprazole impurity a and lansoprazole nitrogen oxide impurity are not completely separated.
Example 8
The embodiment discloses a method for separating and detecting lansoprazole nitrogen oxide impurities.
The difference from example 5 is that: the injection volume was 20 ul.
The HPLC profile was observed, see FIG. 8: three base peaks exist on the map, and the peaks of lansoprazole impurity A and lansoprazole nitrogen oxide impurity are not completely separated.
Example 9
The embodiment discloses a method for separating and detecting lansoprazole nitrogen oxide impurities.
The difference from example 5 is that: the pH of the mobile phase BD was adjusted to 7.3 with phosphoric acid solution (1 → 10), the detection wavelength was 284nm, the injection volume was 10. mu.l, the column temperature was 25 ℃ and the elution gradient was as follows:
the HPLC profile was observed, see FIG. 9: two base peaks exist on the map, and the peaks of lansoprazole impurity A and lansoprazole nitrogen oxide impurity are not completely separated.
Example 10
The embodiment discloses a method for separating and detecting lansoprazole nitrogen oxide impurities.
The difference from example 5 is that: the mobile phase B is a mixture of 100: 450: 4.5: 1.0 methanol-water-triethylamine-phosphoric acid solution
The HPLC profile was observed, see FIG. 10: two base peaks exist on the map, and the peaks of lansoprazole impurity A and lansoprazole nitrogen oxide impurity are not completely separated.
Example 11
The embodiment discloses a method for separating and detecting lansoprazole nitrogen oxide impurities.
The difference from example 5 is that: the mobile phase B is a mixture of 100: 500: 5.0: 1.5 methanol-water-triethylamine-phosphoric acid solution the HPLC profile was observed, see FIG. 11: the retention time of the lansoprazole impurity A is 5.873min, and the retention time of the lansoprazole nitrogen oxide impurity is 6.801 min.
Example 12
The embodiment discloses a method for separating and detecting lansoprazole nitrogen oxide impurities.
The difference from example 5 is that: the mobile phase B is a mixture of 100: 550: 6.0: 2.0 methanol-water-triethylamine-phosphoric acid solution.
The HPLC profile was observed, see FIG. 12: the retention time of the lansoprazole impurity A is 6.333min, and the retention time of the lansoprazole nitrogen oxide impurity is 7.283 min.
Example 13
The embodiment discloses a method for separating and detecting lansoprazole nitrogen oxide impurities.
The difference from example 12 is that: the column temperature was 20 ℃.
Observe the HPLC profile, see fig. 13: two base peaks exist on the map, and the peaks of lansoprazole impurity A and lansoprazole nitrogen oxide impurity are not completely separated.
Example 14
The embodiment discloses a method for separating and detecting lansoprazole nitrogen oxide impurities.
The difference from example 12 is that: the column temperature was 30 ℃.
Observe the HPLC profile, see fig. 14: two base peaks exist on the map, and the peaks of lansoprazole impurity A and lansoprazole nitrogen oxide impurity are not completely separated.
Example 15
The embodiment discloses a method for separating and detecting lansoprazole nitrogen oxide impurities.
The difference from example 12 is that: the column temperature was 40 ℃.
Observe the HPLC profile, see fig. 15: two base peaks exist on the map, and the peaks of lansoprazole impurity A and lansoprazole nitrogen oxide impurity are not completely separated.
Comparative example
The relevant substance detection standard of lansoprazole impurity A raw material is recorded in second part of pharmacopoeia of 2020 edition of Chinese pharmacopoeia, octadecylsilane chemically bonded silica is used as a filler (4.6mm multiplied by 250mm, 5 μm), a methanol-water-triethylamine-phosphoric acid volume ratio (600: 400: 5: 1.5) [ a pH value is adjusted to 7.3 by a phosphoric acid solution (1 → 10) ] is used as a mobile phase, and the detection wavelength is 284 nm.
Taking about 10mg of lansoprazole impurity A and about 10mg of m-chloroperoxybenzoic acid, placing the lansoprazole impurity A and the m-chloroperoxybenzoic acid into the same 20ml measuring flask, adding a methanol-water (60: 40) solution to dissolve and dilute to a scale, placing for 10 minutes, taking 10 microlitres to inject into a liquid chromatograph, and adjusting the proportion of a mobile phase to ensure that the retention time of the lansoprazole impurity A peak is about 10 minutes, and the lansoprazole impurity A peak and the lansoprazole nitrogen oxide impurity are obtained.
And (4) observing an HPLC (high performance liquid chromatography) spectrum, wherein the lansoprazole nitrogen oxide and the lansoprazole impurity A in the figure 16 can not be separated completely, and only one peak is formed finally.
The result of the detection
The retention time, resolution R ═ 2 (difference in retention time/sum of widths of two peaks) according to the HPLC profiles of examples 1 to 15 and comparative example 1 are collated in table 6.
TABLE 6
According to the comparison of the data of comparative example 1 and example 1 in table 6, the baseline of lansoprazole impurity a and nitrogen oxide impurity in example 1 is completely separated, the separation degree reaches 0.66, while the two peaks in comparative example 1 coincide and do not reach the state of starting separation, which shows that the separation degree between two impurities is increased by using octadecylsilane bonded silica gel as the stationary phase and methanol-water-triethylamine-phosphoric acid solution as the mobile phase and performing elution according to the elution gradient of the application, so that the retention time of lansoprazole impurity a and lansoprazole nitrogen oxide impurity can be increased, thereby reflecting the real main peak and realizing the effective separation detection of impurity a and nitrogen oxide impurity. A method for accurately detecting the lansoprazole nitrogen oxide impurities is developed, the technical gap of the lansoprazole nitrogen oxide impurity detection is filled, and the quality control and influence on the raw material of the lansoprazole nitrogen oxide impurities A and the preparation thereof are profound.
According to the comparison of the data of examples 1 and 4 and examples 2 and 5 in table 6, the degrees of separation of examples 2 and 5 are both greater than those of examples 1 and 4, which shows that the elution gradients are further selected such that the volume of mobile phase a at 0min accounts for 45% of the column volume, the volume of mobile phase B accounts for 55% of the column volume, the volume of mobile phase a at 20min accounts for 45-50% of the column volume, the volume of mobile phase B accounts for 50-55% of the column volume, the volume of mobile phase a at 40min accounts for 60% of the column volume, and the volume of mobile phase B accounts for 40% of the column volume, so that the retention time difference between lansoprazole impurity a and lansoprazole nitrogen oxide impurity is further large, the degree of separation between the two impurities is further increased to reflect a more real main peak, the two impurities can be better separated, and thus more accurate purity of lansoprazole is obtained to better control the quality of the pharmaceutical substances.
As can be seen from comparison of the data in table 6 in examples 1, 2, 4 and 5 with example 3, the separation degree in example 5 is greater than that in examples 1, 2, 4 and 5, which shows that the mobile phase a volume at 0min of the elution gradient accounts for 35%, the mobile phase B volume accounts for 65%, the mobile phase a volume at 20min accounts for 45%, the mobile phase B volume accounts for 55%, the mobile phase a volume at 40min accounts for 55%, and the mobile phase B volume accounts for 45%, so that the separation degree of lansoprazole impurity a and lansoprazole nitrogen oxide impurity is maximized under the condition of only adjusting the mobile phase volume, thereby obtaining more accurate purity of lansoprazole.
As can be seen from a comparison of the data in table 6 for examples 11-12 and example 5, the separation degrees for examples 11-12 are all greater than for example 5, indicating that the volume ratio of methanol-water-triethylamine-phosphoric acid in mobile phase B is 100: (550-550): (5.0-6.0): (1.5-2.0), the mobile phase is used for better distinguishing the lansoprazole nitrogen oxide impurities from the lansoprazole impurities A, so that more accurate purity of the lansoprazole can be obtained.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (10)
1. A method for separating lansoprazole nitrogen oxide impurities is characterized by comprising the following steps: using octadecylsilane chemically bonded silica as a stationary phase, using a mobile phase A and a mobile phase B as mobile phases, and detecting by adopting a reversed-phase high performance liquid chromatography to control a sample, wherein the sum of the volume ratio of the mobile phase A to the mobile phase B is 100%, the polarity of the mobile phase is greater than that of the stationary phase, the mobile phase A is methanol, and the volume ratio of the mobile phase B is 100: (440-550): (4.4-6.0): (0.9-2) eluting with a methanol-water-triethylamine-phosphoric acid solution according to the following elution gradient:
。
2. The process for the separation of lansoprazole nitrogen oxide impurity of claim 1, wherein: the elution gradient was:
。
3. The process for the separation of lansoprazole nitrogen oxide impurity of claim 1, wherein: the elution gradient was:
。
4. The process for the separation of lansoprazole nitrogen oxide impurity according to any one of claims 1-3, characterized in that: the pH value of the mobile phase B is 7.1-7.5.
5. The process for the separation of lansoprazole nitrogen oxide impurity of claim 4, wherein: the volume ratio of the methanol to the water to the triethylamine to the phosphoric acid is 100: (500-550): (5.0-6.0): (1.5-2.0).
6. The process for the separation of lansoprazole nitrogen oxide impurity of claim 4, wherein: the volume ratio of the methanol to the water to the triethylamine to the phosphoric acid is 100: 440: 4.4: 0.9.
7. a method for detecting lansoprazole nitrogen oxide impurities is characterized by comprising the following steps: and (3) putting the sample solution into a high performance liquid chromatography tester, wherein the sample injection volume is 5ul during testing.
8. The method for detecting the lansoprazole nitrogen oxide impurity according to claim 7, wherein: the column temperature during the test is 32-38 ℃.
9. The method for detecting the lansoprazole nitrogen oxide impurity according to claim 7, wherein: the column temperature was 35 ℃ when tested.
10. The method for detecting the lansoprazole nitrogen oxide impurity according to claim 9, wherein: the detection wavelength is 284nm, and the operation is carried out in a dark place.
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