Method for removing residual water-soluble organic solvent in sample
An organic solvent and water-soluble technology, which is applied in the field of removal of residual water-soluble organic solvents in samples, can solve problems such as inability to remove organic solvents, and achieve high removal efficiency
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Embodiment 1
[0018] Such as figure 1 As shown, the removal of residual ethanol in the drug is carried out according to the following process:
[0019] 1) Mixing of ammonium chloride besylate and deionized water containing 5% ethanol: add deionized water to the sample at a ratio of 1:10 (weight ratio), and stir fully at 25 degrees Celsius to make the sample and water fully mix.
[0020] 2) Add a hydroxyphenol additive with a weight ratio of 1:100 ortho-alkyl chain length of 2 to the sample and water mixture to precipitate the sample from the solution;
[0021] 3) Centrifuge the precipitated sample at a speed of 1000 rpm, and collect the precipitated sample after centrifugation for 5 minutes;
[0022] 4) For the precipitated sample, use headspace gas chromatography to measure the residual ethanol content therein; if the content meets the requirements, then end the freeze-drying; otherwise, repeat the above steps 1-3 until the residual ethanol mass content in the sample is less than 0.6 %....
Embodiment 2
[0024] Such as figure 1 As shown, the removal of residual acetone in the drug is carried out according to the following process:
[0025] 1) Mixing of the drug amoxicillin containing 1% acetone and deionized water: add deionized water to the sample according to the ratio of 1:5 (weight ratio), stir well at 30 degrees Celsius (so that the sample and water are fully mixed .
[0026] 2) Add a hydroxyphenol additive with a meta-alkyl chain length of 4 in a weight ratio of 1:50 to the sample and water mixture to precipitate the sample from the solution;
[0027] 3) Centrifuge the precipitated sample at a speed of 2000 rpm to collect the precipitated sample;
[0028] 4) For the precipitated sample, use headspace gas chromatography to measure the residual acetone content therein; if the content meets the requirements, then end the freeze-drying; otherwise, repeat the above steps 1-3 until the residual acetone mass content in the sample is less than 0.1 %.
Embodiment 3
[0030] Such as figure 1 As shown, the removal of residual methanol in the drug is carried out according to the following process:
[0031] 1) Mixing of vitamin E containing 0.5% methanol and deionized water: add deionized water to the sample at a ratio of 1:20 (weight ratio), and ultrasonically operate at 45 degrees Celsius to fully mix the sample and water.
[0032] 2) Add a hydroxyphenol additive with a para-alkyl chain length of 6 in a weight ratio of 1:20 to the mixture of the sample and water to precipitate the sample from the solution;
[0033] 3) Centrifuge the precipitated sample at a speed of 4000 rpm, and collect the precipitated sample after centrifugation for 30 minutes;
[0034] 4) For the precipitated sample, use headspace gas chromatography to measure the residual methanol content therein; if the content meets the requirements, then end the freeze-drying; otherwise, repeat the above steps 1-3 until the residual methanol mass content in the sample is less than 0...
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