Assay
Internal standard solution
Dissolve about 500mg of 4-tert-butylphenol,accurately weighed,in acetone in a 100-mLvolumetric flask,add acetone to volume,and mix.
Standard preparation
Dissolve accurately weighed quantities of USP3-tert-Butyl-4-hydroxyanisole RSand USP2-tert-Butyl-4-hydroxyanisole RSin Internal standard solutionto obtain a solution having known concentrations of about 9mg per mLand about 1mg per mL,respectively.
Assay preparation
Dissolve about 100mg of Butylated Hydroxyanisole,accurately weighed,in Internal standard solutionin a 10-mLvolumetric flask,dilute with Internal standard solutionto volume,and mix.
Chromatographic system (see Chromatography á621ñ)
The gas chromatograph is equipped with a flame-ionization detector,and contains a 2-mm ×1.8-m stainless-steel column packed with 10%liquid phase G26on support S1A.The carrier gas is helium.The column is maintained isothermally at a temperature between 175

and 185

.The injection port temperature is maintained at 200

,and the detector temperature is maintained at about 250

.Chromatograph the
Standard preparation,and record the peak responses as directed for
Procedure:the resolution,
R,between the 3-
tert-butyl-4-hydroxyanisole isomer and the 2-
tert-butyl-4-hydroxyanisole isomer is not less than 1.3;the tailing factor is not more than 2.0;and the relative standard deviation is not more than 2.0%determined from the 3-
tert-butyl-4-hydroxyanisole isomer and not more than 6.0%determined from the 2-
tert-butyl-4-hydroxyanisole isomer.
Procedure
Separately inject equal volumes (about 5µL)of the
Standard preparationand the
Assay preparationinto the gas chromatograph,record the chromatograms,and measure the peak areas for each isomer and the internal standard.Calculate the quantity,in mg,of each isomer in the portion of Butylated Hydroxyanisole taken by the formula:
10C(RU/RS),
in which
Cis the concentration,in mg per mL,of the appropriate USP Reference Standard;and
RUand
RSare the peak area ratios of the corresponding isomer to the internal standard obtained from the
Assay preparationand the
Standard preparation,respectively.Calculate the weight,in mg,of C
11H
16O
2in the portion of Butylated Hydroxyanisole taken by adding the quantities of the two isomers.