Limit of potassium
[NOTEThe
Standard solution and the
Test solutions may be modified, if necessary, to obtain solutions of suitable concentrations, adaptable to the linear or working range of the instrument.
]
Standard solution
Transfer 5.959 g of potassium chloride, previously dried at 105
for 2 hours and accurately weighed, to a 250-mL volumetric flask, dilute with water to volume, and mix. This solution contains 12.5 mg of potassium per mL. Dilute an accurately measured volume of this solution quantitatively, and stepwise if necessary, with water to obtain a solution containing 31.25 µg of potassium per mL.
Test solutions
Transfer 62.5 mg of Levocarnitine to a 100-mL volumetric flask, dissolve in and dilute with water to volume, and mix to obtain a stock solution. To three separate 25-mL volumetric flasks add 0, 2.0, and 4.0 mL of the Standard solution. To each flask add 20.0 mL of the stock solution, dilute with water to volume, and mix. These solutions contain 0 (Test solution A), 2.5 (Test solution B), and 5.0 (Test solution C) µg per mL of potassium.
Procedure
Concomitantly determine the absorbances of the
Test solutions at the potassium emission line at 766.7 nm with a suitable atomic absorption spectrophotometer (see
Spectrophotometry and Light-Scattering 851) equipped with an airacetylene flame, using water as the blank. Plot the absorbances of the
Test solutions versus their contents of potassium, in µg per mL, draw the straight line best fitting the three points, and extrapolate the line until it intercepts the concentration axis. From the intercept determine the amount, in µg, of potassium in each mL of
Test solution A. Calculate the percentage of potassium in the portion of Levocarnitine taken by multiplying the concentration, in µg per mL, of potassium found in
Test solution A by 0.2: not more than 0.2% is found.
Limit of sodium
[NOTEThe
Standard solution and the
Test solutions may be modified, if necessary, to obtain solutions of suitable concentrations, adaptable to the linear or working range of the instrument.
]
Standard solution
Transfer 6.355 g of sodium chloride, previously dried at 105
for 2 hours and accurately weighed, to a 250-mL volumetric flask, dilute with water to volume, and mix. This solution contains 10.0 mg of sodium per mL. Dilute an accurately measured volume of this solution quantitatively, and stepwise if necessary, with water to obtain a solution containing 250 µg of sodium per mL.
Test solutions
Transfer 4.0 g of Levocarnitine to a 100-mL volumetric flask, dissolve in and dilute with water to volume, and mix to obtain a stock solution. To three separate 25-mL volumetric flasks add 0, 2.0, and 4.0 mL of the Standard solution. To each flask add 20.0 mL of the stock solution, dilute with water to volume, and mix. These solutions contain 0 (Test solution A), 20.0 (Test solution B), and 40.0 (Test solution C) µg per mL of sodium.
Procedure
Concomitantly determine the absorbances of the
Test solutions at the sodium emission line at 589.0 nm with a suitable atomic absorption spectrophotometer (see
Spectrophotometry and Light-Scattering 851) equipped with an airacetylene flame, using water as the blank. Plot the absorbances of the
Test solutions versus their contents of sodium, in µg per mL, draw the straight line best fitting the three points, and extrapolate the line until it intercepts the concentration axis. From the intercept determine the amount, in µg, of sodium in each mL of
Test solution A. Calculate the percentage of sodium in the portion of Levocarnitine taken by multiplying the concentration, in µg per mL, of sodium found in
Test solution A by 0.003125: not more than 0.1% is found.
Assay
Transfer about 100 mg of Levocarnitine, accurately weighed, to a 250-mL flask, and dissolve in a mixture of 3 mL of formic acid and 50 mL of glacial acetic acid. Add 2 drops of
crystal violet TS, and titrate with 0.1 N perchloric acid VS to an emerald green endpoint. Perform a blank determination, and make any necessary correction. Each mL of 0.1 N perchloric acid is equivalent to 16.12 mg of C
7H
15NO
3.