Method for determining related substances of propofol tenofovir by high performance liquid chromatography
A technology of tenofovir and related substances, applied in the field of drug analysis, can solve the problems of difficult separation of by-products such as diastereoisomers and undetected potential impurities, so as to shorten the elution time, ensure safe drug use, and generality high effect
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experiment example 1
[0039] Experimental example 1 System suitability inspection
[0040] Take an appropriate amount of impurity 1-11 reference substance and tenofovir alafenamide (TAF) reference substance, add phase A to dissolve and quantitatively dilute to form a mixed solution, wherein the final mixture of impurities 1-7 and tenofovir alafenamide The concentration was 2 μg / ml, and the final concentration of impurities 8-11 was 1 μg / ml, as a system suitability solution.
[0041] Take the system suitability solution and inject it into the liquid chromatograph, and the chromatographic conditions are as follows:
[0042] Chromatographic column: Thermo Hypersil BDS C18 (250mm×4.6mm, 5μm)
[0043] Phase A: [tetrahydrofuran-acetonitrile (7:3)]-0.02mol / L dipotassium hydrogen phosphate buffer (pH6.0) (1:99)
[0044] Phase B: [tetrahydrofuran-acetonitrile (7:3)]-0.02mol / L dipotassium hydrogen phosphate buffer (pH6.0) (50:50)
[0045] The detection wavelength is 260nm, the flow rate: 1.0ml / min, the ...
Embodiment 2
[0051] Example 2 Other methodological investigations
[0052] (1) Quantitation limit and detection limit
[0053] The limit of quantification and detection sensitivity of TAF and each impurity all meet the requirements (see Table 4).
[0054] Table 4
[0055]
[0056]
[0057] (2) Linearity and range
[0058] Within the specified measurement range (impurity 1-3, 5, 8-11: 1-30μg / ml, impurity 4: 1-32μg / ml, impurity 6-7: 0.8-24μg / ml, TAF: 0.9-27μg / ml ), the peak area of TAF and each impurity has a good linear relationship with the concentration, and r is greater than 0.99.
[0059] (3) Precision and repeatability
[0060] 6 samples were prepared in parallel by 2 different experimenters for detection. The RSDs with impurity content > 0.1% were all less than 20%, and the RSDs with impurity content ≤ 0.1% were all less than 50%. The detection method of the present invention has good precision and repeatability .
[0061] (4) Recovery rate and accuracy
[0062] The r...
Embodiment 3
[0069] Example 3 Detection of related substances in TAF samples
[0070] Three batches of TAF samples were synthesized by the synthesis method in CHAPMAN et al. (Nucleosides and Nucleic Acids, 20(4-7):621-628, 20010401) as samples to be tested.
[0071] Accurately weigh an appropriate amount of the sample to be tested, add phase A to dissolve and quantitatively dilute to make a 1mg / ml solution as the test solution. Precisely measure an appropriate amount of the test solution, and quantitatively dilute it with phase A to make a 1 μg / ml solution as a control solution.
[0072] Accurately measure control solution and need testing solution, inject liquid chromatograph, adopt chromatographic condition 1 and chromatographic condition 2 in Table 6 to detect respectively, and the results are shown in Table 7.
[0073] Table 6 Chromatographic conditions
[0074]
[0075]
[0076] Table 7
[0077]
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