Method for detecting genotoxic impurity in gatiated cyclized ester
A technology for adding and replacing cyclic esters and a detection method, which is applied in the directions of measuring devices, instruments, scientific instruments, etc., can solve problems such as blockage of chromatographic columns and pressure rise, and achieve the effect of solving blockage of chromatographic columns.
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Embodiment 1
[0058] Embodiment 1 detection method
[0059] (1) Instrument conditions and reagents
[0060] Instruments and conditions: ultra-high performance liquid chromatography-tandem mass spectrometer: model: Agilent1290&Agilent QQQ, AgilentQQQ equipped with ESI (+) MS detector; column: Agilent Eclipse Plus C18 RRHD 3.0×150mm, 1.8µm; Agilent Eclipse Plus C18 RRHD 3.0 ×150mm, 1.8µm, electronic analytical balance, gradient elution conditions are shown in Table 1, mass spectrometer conditions are shown in Table 2.
[0061] Reagents and reference substances: methanol: HPLC; ultrapure water: HPLC; formic acid: HPLC; acetonitrile: HPLC; intermediate A1: content 99.5%; moxifloxacin S1: NA.
[0062] (2) Test operation
[0063] ① Solution preparation:
[0064] Diluent: acetonitrile;
[0065] Blank solution: diluent;
[0066] Intermediate A1 stock solution: Accurately weigh about 20mg of the intermediate A1 reference substance and place it in a 200ml volumetric flask, add diluent to dissolv...
Embodiment 2
[0077] Embodiment 2 System Applicability
[0078] The system suitability is realized by the RSD of the peak area of intermediate A1 in the 5-pin reference solution. It is required that the RSD of the peak area of intermediate A1 in the 5-pin reference solution should not be greater than 10.0%.
[0079] (1) Solution preparation
[0080] 1) Diluent: acetonitrile;
[0081] 2) Blank solution: diluent;
[0082] 3) Preparation of intermediate A1 stock solution: refer to the preparation of intermediate A1 stock solution in Example 1, and the obtained concentration is 98.1568 ng / ml;
[0083] 4) Reference solution preparation: refer to the preparation of the reference solution in Example 1, and the obtained concentration is 2.9447ng / ml;
[0084] (2) Sample injection
[0085] After the system was stabilized, according to the detection method of Example 1, 5 injections of the reference solution were injected, and the spectra were recorded.
[0086] The measurement results:
[0...
Embodiment 3
[0088] Example 3 specificity
[0089] Specificity is achieved by determining whether the blank solution interferes with the detection of intermediate A1; before and after sample addition, the separation and recovery of intermediate A1 in the selective solution. It is required that the blank solution should not interfere with the detection of intermediate A1; the separation between intermediate A1 and adjacent peaks in the selective solution should not be less than 1.5; before and after adding samples, the recovery rate of intermediate A1 in the selective solution should be 70.0%~ Between 130.0%.
[0090] (1) Solution preparation
[0091] 1) Diluent: acetonitrile;
[0092] 2) Blank solution: diluent;
[0093] 3) Intermediate A1 stock solution: see the intermediate A1 stock solution under system suitability in Example 2;
[0094] 4) Intermediate A1 positioning solution (reference solution): see the reference solution under system suitability in Example 2;
[0095] 5) Moxifl...
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