A method for simultaneous determination of butylphthalide and its related substances
A technology related to substances and butylphthalide, which is applied in the field of drug analysis, can solve problems such as separation difficulties, and achieve the effects of good specificity, improved work efficiency, and good repeatability
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Embodiment 1
[0077] The determination of embodiment 1 detection wavelength
[0078] Preparation of diluent: Measure 400mL of acetonitrile and 600mL of water, stir and mix evenly, the obtained solution is also a blank solution, use a UV spectrophotometer to measure the maximum absorption wavelength of each impurity and butylphthalide reference substance, see the results in Figure 1-7 .
[0079] Scan the spectrum by full wavelength Figure 1-7 , Butylphthalide and its various impurities have relatively large absorption at a wavelength of about 226-230nm, and the preferred wavelength is 228nm, so the detection wavelength is determined to be 228nm.
Embodiment 2
[0080] Embodiment 2 system suitability experiment
[0081] Chromatographic conditions: Shimadzu LC-20A or Dionne U3000 high-performance liquid chromatography system and workstation; automatic sample injection; Welch Ultimate XB C 18 (4.6mm×250mm, 5μm) is a separation column; UV detection wavelength: 228nm; mobile phase: 0.2% disodium hydrogen phosphate solution and acetonitrile (gradient elution); column temperature 25°C, injection volume 20μL, flow rate 1.0mL / min;
[0082] gradient program
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[0084]
[0085] Preparation of positioning solution:
[0086] Weigh about 25mg of phthalic acid, weigh it accurately, put it in a 50mL measuring bottle, add diluent to dissolve and dilute to the mark, shake well, weigh 200μL of the solution, put it in a 20mL volumetric flask, and obtain a concentration of 5μg / mL Phthalate positioning solution;
[0087] Weigh about 25 mg of Intermediate I, weigh it accurately, put it in a 50 mL volumetric flask, add diluent to dissolve ...
Embodiment 3
[0107] Embodiment 3 specificity test
[0108] Investigate the degradation research of butylphthalide bulk drug, the forced degradation conditions include acid, alkali, oxidation, high temperature and light, the specific degradation test is as follows:
[0109] Undamaged sample: Take about 25mg of butylphthalide raw material, weigh it accurately, put it in a 50mL measuring bottle, add diluent to dissolve and dilute to the mark, shake well, and you get it.
[0110] Acid destruction: Take about 25mg of butylphthalide raw material, weigh it accurately, put it in a 50mL measuring bottle, add 2mL of 1mol / L hydrochloric acid solution to destroy it for 6 hours; add an equal amount of 1mol / L sodium hydroxide solution to neutralize, add dilution Dissolve the agent and dilute to the mark, shake well, and you have it.
[0111] Alkali destruction: Take about 25mg of butylphthalide raw material, weigh it accurately, put it in a 50mL measuring bottle, add 2mL of 1mol / L sodium hydroxide solu...
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