Phthalimide Potassium Salt CAS 1074-82-4 Purity >99.0% (HPLC)

3. Test method
3.1 Loss on Drying (W/W)
3.1.1 Equipment and instruments
One over ten thousand of electronic balance, electric thermostatic drying oven, 40*25 weighing bottle, dryer
Reagent: silica gel
3.1.2 Methods
1. Clean 3 40*25 weighing bottles.
2, put in the oven at 105℃ (±2℃) dry for 1 hour.
3. Take out the 40*25 weighing bottle and put it into the dryer to cool for 30min.
4, Accurate weighing 40*25 measuring bottle empty weight W0.
5. Use a 40*25 weighing bottle to weigh the evenly mixed sample of 3.0000g (W1), a total of 3.
6, Put in the oven, take off the bottle cap, put it next to the weighing bottle, or half open the bottle cap for drying, take out, must be good weighing bottle cap, dry at 105℃ (±2℃) for 3 hours.
7. Take out the 40*25 weighing bottle and put it into the drying device to cool for 30min.
8, Accurate weighing after drying 40*25 weight of the bottle W2.
Calculation formula: Loss on Drying (%) =(W1-W2)/(W1-W0)×100%
3. 4 Content determination
3.4.1 Instruments and equipment
LC-UV100 Liquid Chromatograph (Shanghai Wufeng Scientific Instrument Co., LTD.)
10ml volumetric bottle, stainless steel corner spoon and other related facilities
3.3.2 Methods
Method for analysis of Phthalimide Potassium Salt
3.3.3 Liquid chromatography
Chromatographic condition
Chromatographic column: HypersilC6H5 (C8 also available) 4.6*250mm 5um
Detection wavelength: 210nm
Column temperature: 30℃
Flow rate: 1.0ml/min
Sample concentration: 0.05mg/ml (diluent is the mobile phase)
Reagents
Potassium Phosphate Dibasic(analytical pure)
Phthalimide Potassium Salt (standard sample)
Acetonitrile (analytical pure)
Pure water
Mobile phase: acetonitrile: phosphate buffer (PH:3.5) =40:60
Weigh 1.63g Potassium Phosphate Dibasic and dissolve in 600ml pure water, adjust the PH value to 3.5 with phosphoric acid, pour into 1000ml beaker containing 400ml acetonitrile, mix well, filter with 0.45um mixed fiber filter membrane, dissolve with ultrasonic vibration, and standby application.
3.3.4 Procedure
1) Configuration test solution (0.05mg/ml)
The 2.5mg sample was accurately weighed and put into a 50ml volumetric bottle. The mobile phase was added and diluted to the scale by ultrasonic dissolution.
2) Configuration standard solution (1.0mg/ml)
The 2.5mg standard sample was accurately weighed and put into a 50ml volumetric bottle. The mobile phase was added and diluted to the scale by ultrasonic dissolution.
3) System usability:
(1) Put the filter head into 80% methanol at startup, open the exhaust valve and drain for 3-5min, and close the exhaust valve and rinse for 10-15min. Then put the filter head into 90% pure water, open the drain valve and drain for 3-5min, close the drain valve and rinse for 10min.
(2) Then change the prepared mobile phase, the flow rate is 1.0ml/min, the column front pressure is less than 1000Psi, open the detector, wait until the column front pressure is stable, open the computer workstation, and enter online
(3) After the column front pressure is stable, open the detector. First inject 1 needle of mobile phase, then inject 1 needle of standard sample, and finally inject sample.
(4) Calculation results: area normalization method
(5) After finishing the analysis task, close the detector first, and then rinse the filter head in pure water for 10-15min; At the same time, the injection valve was rinsed with water and methanol.
(6) Finally, put on 80% methanol, rinse for 30min, and shut down.
4. After completion of inspection, fill in the inspection and laboratory test sheet.