Assay
Sodium perchlorate buffer
Prepare a 0.14Msolution of sodium perchlorate in water,and adjust with 10Nsodium hydroxide or 0.05Mphosphoric acid to a pHof 3.0.
Mobile phase
Prepare a filtered and degassed mixture of
Sodium perchlorate bufferand acetonitrile (69:31).Make adjustments if necessary (see
System Suitabilityunder
Chromatography á621ñ).
Standard preparation
Dissolve an accurately weighed quantity of
USP Gallamine Triethiodide RSin
Mobile phase,and dilute quantitatively,and stepwise if necessary,with
Mobile phaseto obtain a solution having a known concentration of about 1.0mg per mL.
Assay preparation
Transfer about 25mg of Gallamine Triethiodide,accurately weighed,to a 25-mLvolumetric flask,dissolve in and dilute with Mobile phaseto volume,and mix.
Chromatographic system
(see
Chromatography á621ñ)The liquid chromatograph is equipped with a 200-nm detector and a 4.6-mm ×25-cm column that contains packing L1.The flow rate is about 1.0mLper minute.Chromatograph the
Standard preparation,and record the peak responses as directed under
Procedure:the column efficiency is not less than 5000theoretical plates,the tailing factor is not more than 1.4,and the relative standard deviation for replicate injections is not more than 2.0%.
Procedure
Separately inject equal volumes (about 10µL)of the
Standard preparationand the
Assay preparationinto the chromatograph,record the chromatograms,and measure the responses for the major peaks.Calculate the quantity,in mg,of C
30H
60I
3N
3O
3in the portion of Gallamine Triethiodide taken by the formula:
25C(rU/rS),
in which
Cis the concentration,in mg per mL,of
USP Gallamine Triethiodide RSin the
Standard preparation,and
rUand
rSare the peak responses obtained from the
Assay preparationand the
Standard preparation,respectively.