In recent years, the growing demand of the biopharmaceutical industry, so that the industry as a whole is in the fast lane of sustained and rapid development, the future will usher in the peak period of biological drug listing, the space is vast, the corresponding life science support industry is also the background of rapid development of Hangzhou micro source detection came into being, today for everyone to introduce the identification of defoamer residue detection in RAW Materials verification.
Defoamer is an important part of the biopharmaceutical process, and most of the purpose relies on foreign imports, in recent years, in order to meet the requirements of supervision, it is necessary for us to thoroughly study defoamers, including the ingredients of defoamers, the detection of defoamer residues in APIs, and do a good job in related control work.
At present, the mainstream defoamer in the industry is silicone defoamer, and the micro-source detection laboratory has done a lot of preliminary work and developed a set of gas methods for detecting defoamer residues in APIs.
What are the main components of silicone defoamers analyzed by micro-source detection:
Hexamethylcyclotrisiloxane
Octamethylcyclotetrasiloxane
Decamethylcycloopentasiloxane
Dodecylcyclohexasiloxane and the like
Experimental procedure:
Sample preparation:
Take 2 ml blank (water), sample, add 6 ml pure water and 5 ml solvent, shake for 2 min;
After letting stand for two minutes, add 2 ml of acetonitrile and take the upper organic phase in a nitrogen blowpipe;
Add 8 ml of solvent to repeated extraction once, merge the organic phase twice;
Add 500ul working solution to the nitrogen blowpipe;
Nitrogen is concentrated to less than 2 ml, the volume is set with a solvent to a scale of 1 ml, and it is analyzed on the machine.
Sample analysis:
Sample analysis method:
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Gas phase method
Columns
**************************
Injection volume
1st
Carrier gas
he
velocity of flow
1.5ml/min
Shunt mode and shunt ratio
No shunting
Heating program
Start at 40 °C, heat up to 240 °C at 20 °C/ min, hold for 15 min
Mass spectrometry methods
ms ion source temperature
no,230°C
ms Quad rod temperature
150℃
Mass spectrometry scanning mode
yes
Solution preparation:
Diluent: ethanol
Blank solution: ethanol
Control stock solution: cancel the foaming agent 40 mg, precise weighing, put 20 ml measuring bottle, dilute with diluent to scale, shake well; pipette 1ml of the above solution in 20 ml measuring bottle, dilute with diluent to scale, shake well, as defoamer stock solution.
Control solution: take 1 ml of control stock solution with precision, place 5 ml centrifuge tube, add 1 ml of diluent, shake well.
Sample solution: Take 100 mg of sample, weigh it precisely, place a 5 ml centrifuge tube, add 2 ml of diluent, and shake well.
30% linear solution: take 0.3 ml of the control stock solution with precision, place a 5 ml centrifuge tube, add 1.7 ml of diluent, shake well.
50% linear solution: take 0.5 ml of the control stock solution with precision, place a 5 ml centrifuge tube, add 1.5 ml of diluent, and shake well.
80% linear solution: take 0.8 ml of the control stock solution with precision, place a 5 ml centrifuge tube, add 1.2 ml of diluent, shake well.
100% linear solution: take 1 ml of control stock solution, place 5 ml centrifuge tube, add 1 ml of diluent, shake well.
150% linear solution: take 1.5 ml of the control stock solution, place a 5 ml centrifuge tube, add 0.5 ml of diluent, and shake well.
200% linear solution: i.e. control stock solution
The detection limit of defoamer (bubble enemy) under this method can reach about 10 ppm, which needs to be determined according to the solubility of the sample.
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