Method for detecting valeryl chloride in valsartan
A technology of n-valeryl chloride and valsartan, applied in the field of drug analysis, can solve problems such as no n-valeryl chloride impurities, and achieve the effects of short time used, good reproducibility and high accuracy
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Embodiment 1
[0049] (1) Instrument conditions and reagents
[0050] Instrument and conditions: ultra-high performance liquid chromatography, column: Agilent Poroshell SB 50mm×4.6mm, 2.7µm; injection volume: 0.2μl; column temperature: 35°C; flow rate: 0.5ml / min; mobile phase A: formic acid : Water = 1:1000 (V / V); mobile phase B: methanol; Agilent QQQ equipped with ESI (+) MS detector, electronic analytical balance.
[0051] The gradient elution conditions are shown in Table 1, and the mass spectrometer conditions are shown in Table 2.
[0052] Reagents and reference substances: formic acid: AR and above; ultrapure water: HPLC; methanol: HPLC; aniline: AR and above; acetonitrile: HPLC;
[0053] (2) Test operation
[0054] ① Diluent: acetonitrile;
[0055] ②Blank solution: diluent;
[0056] ③Sample blank solution: take a 10ml volumetric flask, add 2ml of aniline, add diluent to dilute to the mark, and shake well; accurately measure 1.0ml of the above solution, place it in a 10ml volumetri...
Embodiment 2
[0062] Embodiment 2 System Applicability
[0063] The system suitability is realized by the RSD of the peak area of n-pentanilide in the 5-pin reference solution. It is required that the RSD of the peak area of n-pentanilide in the 5-pin reference solution should not be greater than 10.0%.
[0064] (1) Prepare the solution
[0065] Preparation of n-valeranilide stock solution: prepare the n-valeranilide stock solution with reference to Example 1, and its concentration is 986.3700 ng / ml.
[0066] Preparation of reference solution: reference solution preparation in reference example 1, its concentration is 9.8637 ng / ml;
[0067] (2) Measurement method
[0068] Measure according to the chromatographic conditions of Example 1, inject 5 needles of reference solution, and record the spectrogram.
[0069] (3) Measurement results
[0070]
[0071] Conclusion: The peak area RSD of n-pentanilide in the 5-pin reference solution was 3.8%, which met the standard.
Embodiment 3
[0072] Example 3 Specificity
[0073] Specificity is achieved by determining whether the sample blank solution interferes with the detection of n-valeranilide; before and after adding the sample, the resolution and recovery of n-valeranilide in the selective solution are achieved, requiring the sample blank solution to detect n-valeranilide No interference; the separation between n-pentanilide and adjacent peaks in the selective solution should not be less than 1.5; the recovery rate of n-pentanilide in the selective solution should be between 80.0% and 120.0% before and after adding the sample.
[0074] (1) Prepare the solution
[0075] Preparation of sample blank solution: same as sample blank solution in Example 1.
[0076] Preparation of n-valeranilide localization solution (reference solution): preparation of reference solution in reference example 1, its concentration is 9.8637 ng / ml;
[0077] Preparation of test solution: preparation of test solution in reference exam...
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