|
Halothane
Ethane, 2-bromo-2-chloro-1,1,1-trifluoro-, (±)-. (±)-2-Bromo-2-chloro-1,1,1-trifluoroethane » Halothane contains not less than 0.008 percent and not more than 0.012 percent of thymol, by weight, as a stabilizer.
Packaging and storage
Preserve in tight, light-resistant containers, preferably of Type NP glass, and avoid exposure to excessive heat. Dispense it only in the original container.
Specific gravity
Distilling range, Method II
Refractive index
Acidity or alkalinity
Shake 20 mL with 20 mL of carbon dioxide-free water for 3 minutes, and allow the layers to separate: the aqueous layer requires not more than 0.1 mL of 0.010 N sodium hydroxide or not more than 0.6 mL of 0.010 N hydrochloric acid for neutralization, bromocresol purple TS being used as the indicator.
Water, Method I
Limit of nonvolatile residue
Evaporate 50 mL in a tared dish on a steam bath to dryness, and dry the residue at 105
Chloride and bromide
Shake 25 mL with 25 mL of water for 5 minutes, and allow the liquids to separate completely. Draw off the water layer, and to 10 mL add 1 drop of nitric acid and 5 drops of silver nitrate TS: no opalescence is produced.
Thymol content
Standard thymol solution
Prepare a standard solution of thymol in 0.25 N sodium hydroxide containing 0.1 mg of thymol per mL.
Buffer solution
Use pH 8.0 alkaline borate buffer (see under Solutions in the section Reagents, Indicators, and Solutions).
Chlorimide solution
Dissolve 100 mg of 2,6-dibromoquinonechlorimide in 25 mL of dehydrated alcohol. Prepare a fresh solution for each assay.
Standard thymol curve
Pipet into three 100-mL volumetric flasks 1 mL, 3 mL, and 5 mL, respectively, of Standard thymol solution, and add 0.25 N sodium hydroxide to make the final volume 5.0 mL. Add 5.0 mL of 0.25 N sodium hydroxide to a fourth flask in which the blank is to be prepared. To each flask add 10 mL of Buffer solution, mix by gentle swirling, and add 1 mL of Chlorimide solution. Allow to stand for 15 minutes, accurately timed, add 3 mL of 0.25 N sodium hydroxide to each flask, and add water to volume. With a suitable spectrophotometer, measure the absorbances of the thymol-containing solutions relative to the blank at 590 nm. Plot the readings and draw the curve of best fit.
Procedure
Place about 2 mL of Halothane, accurately weighed, in a 100-mL volumetric flask containing 5 mL of 0.25 N sodium hydroxide, and mix by gentle swirling. Evaporate the halothane under a stream of nitrogen, and add 10 mL of Buffer solution and 1 mL of Chlorimide solution. Swirl gently, allow to stand for 15 minutes, accurately timed, add 3 mL of 0.25 N sodium hydroxide, and add water to volume. Read the absorbance of the resulting solution, and by reference to the Standard thymol curve, calculate the percentage of thymol in the weight of Halothane taken.
Chromatographic purity
Standard preparation
Add 1.0 µL of 1,1,2-trichloro-1,2,2-trifluoroethane to 20.0 mL of the test specimen.
Chromatographic system
Under typical conditions, the gas chromatograph is equipped with a flame-ionization detector, and contains a 3-m × 2-mm stainless steel column packed with 20% G24 on support S1AB. The column is maintained at 60
Procedure
Inject separately equal volumes (about 2 µL) of the Standard preparation and Halothane into a suitable gas chromatograph, and record the chromatograms. The total area of all peaks (except that of halothane) recorded for the test specimen does not exceed that due to the added 1,1,2-trichloro-1,2,2-trifluoroethane in the Standard preparation (0.005%).
Auxiliary Information
Please check for your question in the FAQs before contacting USP.
Chromatographic Column
USP32NF27 Page 2549
Chromatographic columns text is not derived from, and not part of, USP 32 or NF 27.
|