Method for detecting methyl p-toluenesulfonate and ethyl p-toluenesulfonate in homopiperazine residues
A technology of methyl tosylate and ethyl tosylate, applied in the field of drug quality control, can solve the problems of unpublished detection of homopiperazine and the like, and achieve the effects of simple method and good effect
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0054] In this example, methyl p-toluenesulfonate (MTS) and ethyl p-toluenesulfonate (ETS) were hydrolyzed into p-toluenesulfonic acid under alkaline conditions, and MTS and ETS were indirectly quantified by detecting p-toluenesulfonic acid.
[0055] Accurately weigh 50 mg of this product, put it in a 10 ml measuring bottle, add solvent to dissolve and dilute to the mark, shake well, and use it as the test solution. Precisely weigh about 50 mg of MTS and ETS, put them in 50ml measuring bottles, dissolve them with solvent and dilute to the mark, shake well, take 80 μl each precisely, put them in 20ml measuring bottles, dilute to the mark with solvent and shake well, as Reference substance stock solution; another precision pipette 0.1ml, put in a 10ml measuring bottle, dilute to the mark with a solvent and shake well, as the reference substance solution.
[0056] In this embodiment, several alkaline mobile phases were tried, and the liquid phase conditions in Table 2 below were ...
Embodiment 2
[0066] In the spiked solution with a sample concentration of 10 mg / mL, MTS was hydrolyzed, but ETS was not hydrolyzed. Try to add a certain amount of formic acid to the diluent to adjust the pH of the sample solution, so that the MTS and ETS can maintain their prototypes, inhibit their hydrolysis, and directly detect them. Tried 3 different diluents (i.e. the solvents used to configure the samples), respectively: Diluent 1: 50% H 2 O-50% ACN, Diluent 2: 50% H 2 O-50% ACN-0.1% FA, Diluent 3: 50% H 2 O-50% ACN-0.5% FA, and the detection conditions in Table 4 below are used for detection.
[0067] Table 4
[0068]
[0069] result:
[0070] The chromatogram obtained by using diluent 1 detection is as follows Figure 4-5 As shown, MTS was not detected in the spiked sample, but ETS could be detected; the chromatogram obtained by using diluent 2 was as follows Figure 6-7 As shown, the MTS peak in the spiked sample is very small and can be detected by ETS; Figure 8-9 As sh...
Embodiment 3
[0076] Table 6 shows the detection conditions and results of the pre-validation method for the detection of MTS and ETS residues in homopiperazine.
[0077] Table 6
[0078]
[0079]
[0080] The detected chromatograms are as Figure 10 (STD 40ng / mL) and Figure 11 (100% Spiked 5mg / mL).
[0081] Method Characterization Results:
[0082] 1. Specificity: No interference was observed within the retention time of MTS and ETS.
[0083] 2. Sensitivity solution: MTS: 8ng / mL (1.6ppm), signal-to-noise ratio S / N=54; ETS: 8ng / mL (1.6ppm), signal-to-noise ratio S / N=20.
[0084] 3. Linearity: MTS: 8ng / mL to 80ng / mL (1.6to 16ppm, r=0.9989)
[0085] ETS: 8ng / mL to 80ng / mL (1.6to 16ppm, r = 0.9983)
[0086] 4. Precision:
[0087] MTS:
[0088] % RSD for 6 replicate injections RT 0.1% (n=6);
[0089] % RSD for 6 replicate injections Area 5.6% (n=6)
[0090] ETS:
[0091] % RSD for 6 replicate injections RT 0.2% (n=6);
[0092] % RSD for 6 replicate injections Area 4.3% (n...
PUM
| Property | Measurement | Unit |
|---|---|---|
| Snr | aaaaa | aaaaa |
Abstract
Description
Claims
Application Information
Login to View More