Pramipexole (104632-26-0)

.1. Specification

2. Method of analysis

2.1 Appearance

2.1.1 Take appropriate amount of this product and place it in a clear and colorless glass dish. 2.1.2The result：White or off-white or pale yellow powder.

2.2 Loss on drying

• Dry and clean 50×30mm flat weighing bottle was placed in a drying oven and dried to a constant weight at 105℃. Then, it was taken out and placed in a dryer (with built-in dried silica gel particles) and cooled to room temperature for precise weighing.The product was about 1.0g and placed in the flat weighing bottle with the above constant weight, so that the test product was spread on the bottom of the bottle with a thickness of no more than 5mm. After precise weighing, the product was placed in a drying oven and dried at 105℃ for 3 hours. The product was then taken out and placed in a dryer (with built-in drying silica gel particles) and cooled to room temperature,Its mass is precisely weighed and its drying weight loss is calculated.
• Calculate： Loss on drying= W 2 -W 3 ×100%

W 2 -W1

In this equation：

W1 is the mass of an empty weighing bottle that has been dried to a constant weight,g; W2 refers to the mass of the sample and the weighing bottle before drying,g;

W3 is the mass of the sample and the weighing bottle after drying at 105℃,g.

2.2.3 The result：Loss on drying≤1.0%.

2.3 Residue on ignition

2.3.1 Take a clean crucible and place it in a box-type resistance furnace with constant weight of 500 ~ 600℃ for more than 1 hour. Take it out and place it in a dryer, cool it to room temperature

and weigh it. Then place it in the 600℃ box-type resistance furnace with constant weight for 0.5 hours, take out the cooling and weigh it. If the results show constant weight twice, it can be used; otherwise, continue burning until constant weight.Take samples of 1.0 g, precision said, set on ignition to constant weight in the crucible, slowly on ignition to complete carbonized, let cool to room temperature, add 1 ml humidify sulfate, sulfuric acid clean steam after low temperature heat, let cool to room temperature, in 500 ~ 600 ℃ on ignition completely ashing, displacement in the dryer, let cool to room temperature, precision said later, again in 500 ~ 600 ℃ on ignition to constant weight.

2.3.2 Calculate： Residue on ignition= W3 - W1 ´ 100%

W2 - W1

In this equation：

W1 is the constant weight of the empty crucible, g;

W2 is the total weight of the sample and the constant weight crucible, g; W3 is the total weight of crucible and residue after burning, g.

2.3.3 The result：Residue on ignition≤0.1%.

2.4 Related substances and purity

2.4.1 Chromatographic conditions:

Column：Inertsil ODS-2 C18 column（Octadecyl silane bonded silica gel as the filler）

Flow rate：1.5ml/min Sample quantity：5μl Check wavelength：264nm Column temperature：40℃ Mobile phase A：Buffer

Mobile phase B：Buffer: Acetonitrile（500：500） Elution procedure:

2.4.2 2.4.2

Sample diluent: acetonitrile: buffer (200:800).

Test solution: Put 75mg of this product in 50mL measuring bottle, add sample diluent to dissolve and dilute to scale, shake well to get.

Reference solution (a) : Take the precise amount of the test solution in 1mL to 100ml measuring bottle, add the sample diluent and dilute it to the scale, shake well, and get.

Control solution (B) : 7.5mg of pramipexole system suitable control was weighed and placed in a vial, then the sample diluent was added to dissolve in 5ml and shaken evenly.

2.4.3 Calculate：Self dilution control method

Impurity content=

Test solution impurity peak area Reference solution (a) Impurity peak area ×1000

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