Home >
Community >
The quality standards of amine sulfurine, American Pharmacopoeia, Japanese Pharmacopoeia
Upvote
9
Downvote
+ Chemistry
Posted by
Martin David McCoy
The quality standards of amine sulfurine, American Pharmacopoeia, Japanese Pharmacopoeia
Assay — Solution A-Prepare A 0.005 M SOLUTION of Sodium 1-Octanesulfonate in Dilute Glacial Acetic Acid (1 in 100). Solution b-prepare a mixture of methanol (3 :3: 3: ]Mobile phase— Prepare a mixture of Solution A and Solution B (60:40), filter, and degas. Make adjustments if necessary (see System Suitability under Chromatography 621). Internal standard solution— Transfer 2.0 mL of methylbenzoate to a 100-mL volumetric flask, dilute with methanol to volume, and mix. Standard preparation— Dissolve an accurately weighed quantity of USP Thiamine Hydrochloride RS in Mobile phase to obtain a solution having a known concentration of about 1 mg per mL. Transfer 20.0 mL of this solution to a 50-mL volumetric flask, add 5.0 mL of Internal standard solution, dilute with Mobile phase to volume, and mix to obtain a Standard preparation having a known concentration of about 400 u0026micro;g per mL. [ 123] Assay Preparation -Transfer An Accurately Weighed Quantity ofabout 200 mg of Thiamine Hydrochloride to a 100-mL volumetric flask, dissolve in and dilute with Mobile phase to volume, and mix. Transfer 10.0 mL of this solution to a 50-mL volumetric flask, add 5.0 mL of Internal standard solution, dilute with Mobile phase to volume, and mix. Chromatographic system (see Chromatography 621)—The liquid chromatograph is equipped with a 254-nm detector and a 4-mm × 30-cm column that contains packing L1. The flow rate is about 1 mL per minute. [note—The flow rate may be adjusted as needed to obtain a retention time of about 12 minutes for thiamine hydrochloride. ] Chromatograph the Standard preparation, and record the peak responses as directed for Procedure: the resolution, R , between the thiamine and methylbenzoate peaks is not less than 4.0; the tailing factor for the thiamine peak is not more than 2.0; the column efficiency determined from the thiamine peak is not less than 1500 theoretical plates; and the relative standard deviation for replicate injections is not more than 2.0%. Procedure— Separately inject equal volumes (about 10 u0026micro;L) of the Standard preparation and the Assay preparation into the chromatograph, record the chromatograms, and measure the areas of the major peaks. Calculate the quantity, in mg, of C12H17ClN4OS·HCl in the Thiamine Hydrochloride taken by the formula: 0.5C(RU / RS) in which C is the concentration, in u0026micro;g per mL, of USP Thiamine Hydrochloride RS in the Standard preparation; and RU and RS are the ratios of the peak areas of thiamine to methylbenzoate obtained from the Assay preparation and the Standard preparation, respectively. Auxiliary Information— Please check for your question in the FAQs before contacting USP. Topic/Question Contact Expert Committee Monograph Huy T. Dinh, M.S. Scientific Liaison 1-301-816-8594 (DS2010) Monographs - Dietary Supplements Reference Standards RS Technical Services 1-301-816-8129 rstech@usp.org
Assay — Solution A-Prepare A 0.005 M SOLUTION of Sodium 1-Octanesulfonate in Dilute Glacial Acetic Acid (1 in 100). Solution b-prepare a mixture of methanol (3 :3: 3: ]Mobile phase— Prepare a mixture of Solution A and Solution B (60:40), filter, and degas. Make adjustments if necessary (see System Suitability under Chromatography 621). Internal standard solution— Transfer 2.0 mL of methylbenzoate to a 100-mL volumetric flask, dilute with methanol to volume, and mix. Standard preparation— Dissolve an accurately weighed quantity of USP Thiamine Hydrochloride RS in Mobile phase to obtain a solution having a known concentration of about 1 mg per mL. Transfer 20.0 mL of this solution to a 50-mL volumetric flask, add 5.0 mL of Internal standard solution, dilute with Mobile phase to volume, and mix to obtain a Standard preparation having a known concentration of about 400 u0026micro;g per mL. [ 123] Assay Preparation -Transfer An Accurately Weighed Quantity ofabout 200 mg of Thiamine Hydrochloride to a 100-mL volumetric flask, dissolve in and dilute with Mobile phase to volume, and mix. Transfer 10.0 mL of this solution to a 50-mL volumetric flask, add 5.0 mL of Internal standard solution, dilute with Mobile phase to volume, and mix. Chromatographic system (see Chromatography 621)—The liquid chromatograph is equipped with a 254-nm detector and a 4-mm × 30-cm column that contains packing L1. The flow rate is about 1 mL per minute. [note—The flow rate may be adjusted as needed to obtain a retention time of about 12 minutes for thiamine hydrochloride. ] Chromatograph the Standard preparation, and record the peak responses as directed for Procedure: the resolution, R , between the thiamine and methylbenzoate peaks is not less than 4.0; the tailing factor for the thiamine peak is not more than 2.0; the column efficiency determined from the thiamine peak is not less than 1500 theoretical plates; and the relative standard deviation for replicate injections is not more than 2.0%. Procedure— Separately inject equal volumes (about 10 u0026micro;L) of the Standard preparation and the Assay preparation into the chromatograph, record the chromatograms, and measure the areas of the major peaks. Calculate the quantity, in mg, of C12H17ClN4OS·HCl in the Thiamine Hydrochloride taken by the formula: 0.5C(RU / RS) in which C is the concentration, in u0026micro;g per mL, of USP Thiamine Hydrochloride RS in the Standard preparation; and RU and RS are the ratios of the peak areas of thiamine to methylbenzoate obtained from the Assay preparation and the Standard preparation, respectively. Auxiliary Information— Please check for your question in the FAQs before contacting USP. Topic/Question Contact Expert Committee Monograph Huy T. Dinh, M.S. Scientific Liaison 1-301-816-8594 (DS2010) Monographs - Dietary Supplements Reference Standards RS Technical Services 1-301-816-8129 rstech@usp.org
Solution A-Prepare A 0.005 M SOLUTION of Sodium 1-Octanesulfonate in Dilute Glacial Acetic Acid (1 in 100).
Solution b-prepare a mixture of methanol (3 :3: 3: ]Mobile phase— Prepare a mixture of Solution A and Solution B (60:40), filter, and degas. Make adjustments if necessary (see System Suitability under Chromatography 621).
Internal standard solution— Transfer 2.0 mL of methylbenzoate to a 100-mL volumetric flask, dilute with methanol to volume, and mix.
Standard preparation— Dissolve an accurately weighed quantity of USP Thiamine Hydrochloride RS in Mobile phase to obtain a solution having a known concentration of about 1 mg per mL. Transfer 20.0 mL of this solution to a 50-mL volumetric flask, add 5.0 mL of Internal standard solution, dilute with Mobile phase to volume, and mix to obtain a Standard preparation having a known concentration of about 400 u0026micro;g per mL. [ 123] Assay Preparation -Transfer An Accurately Weighed Quantity ofabout 200 mg of Thiamine Hydrochloride to a 100-mL volumetric flask, dissolve in and dilute with Mobile phase to volume, and mix. Transfer 10.0 mL of this solution to a 50-mL volumetric flask, add 5.0 mL of Internal standard solution, dilute with Mobile phase to volume, and mix.
Chromatographic system (see Chromatography 621)—The liquid chromatograph is equipped with a 254-nm detector and a 4-mm × 30-cm column that contains packing L1. The flow rate is about 1 mL per minute. [note—The flow rate may be adjusted as needed to obtain a retention time of about 12 minutes for thiamine hydrochloride. ] Chromatograph the Standard preparation, and record the peak responses as directed for Procedure: the resolution, R , between the thiamine and methylbenzoate peaks is not less than 4.0; the tailing factor for the thiamine peak is not more than 2.0; the column efficiency determined from the thiamine peak is not less than 1500 theoretical plates; and the relative standard deviation for replicate injections is not more than 2.0%.
Procedure— Separately inject equal volumes (about 10 u0026micro;L) of the Standard preparation and the Assay preparation into the chromatograph, record the chromatograms, and measure the areas of the major peaks. Calculate the quantity, in mg, of C12H17ClN4OS·HCl in the Thiamine Hydrochloride taken by the formula:
0.5C(RU / RS)
in which C is the concentration, in u0026micro;g per mL, of USP Thiamine Hydrochloride RS in the Standard preparation; and RU and RS are the ratios of the peak areas of thiamine to methylbenzoate obtained from the Assay preparation and the Standard preparation, respectively.
Auxiliary Information— Please check for your question in the FAQs before contacting USP.
Topic/Question Contact Expert Committee
Monograph Huy T. Dinh, M.S.
Scientific Liaison
1-301-816-8594 (DS2010) Monographs - Dietary Supplements
Reference Standards RS Technical Services
1-301-816-8129
rstech@usp.org
USP34 – NF29 Page 4408
Solution A-Prepare A 0.005 M SOLUTION of Sodium 1-Octanesulfonate in Dilute Glacial Acetic Acid (1 in 100).
Solution b-prepare a mixture of methanol (3 :3: 3: ]Mobile phase— Prepare a mixture of Solution A and Solution B (60:40), filter, and degas. Make adjustments if necessary (see System Suitability under Chromatography 621).
Internal standard solution— Transfer 2.0 mL of methylbenzoate to a 100-mL volumetric flask, dilute with methanol to volume, and mix.
Standard preparation— Dissolve an accurately weighed quantity of USP Thiamine Hydrochloride RS in Mobile phase to obtain a solution having a known concentration of about 1 mg per mL. Transfer 20.0 mL of this solution to a 50-mL volumetric flask, add 5.0 mL of Internal standard solution, dilute with Mobile phase to volume, and mix to obtain a Standard preparation having a known concentration of about 400 u0026micro;g per mL. [ 123] Assay Preparation -Transfer An Accurately Weighed Quantity ofabout 200 mg of Thiamine Hydrochloride to a 100-mL volumetric flask, dissolve in and dilute with Mobile phase to volume, and mix. Transfer 10.0 mL of this solution to a 50-mL volumetric flask, add 5.0 mL of Internal standard solution, dilute with Mobile phase to volume, and mix.
Chromatographic system (see Chromatography 621)—The liquid chromatograph is equipped with a 254-nm detector and a 4-mm × 30-cm column that contains packing L1. The flow rate is about 1 mL per minute. [note—The flow rate may be adjusted as needed to obtain a retention time of about 12 minutes for thiamine hydrochloride. ] Chromatograph the Standard preparation, and record the peak responses as directed for Procedure: the resolution, R , between the thiamine and methylbenzoate peaks is not less than 4.0; the tailing factor for the thiamine peak is not more than 2.0; the column efficiency determined from the thiamine peak is not less than 1500 theoretical plates; and the relative standard deviation for replicate injections is not more than 2.0%.
Procedure— Separately inject equal volumes (about 10 u0026micro;L) of the Standard preparation and the Assay preparation into the chromatograph, record the chromatograms, and measure the areas of the major peaks. Calculate the quantity, in mg, of C12H17ClN4OS·HCl in the Thiamine Hydrochloride taken by the formula:
0.5C(RU / RS)
in which C is the concentration, in u0026micro;g per mL, of USP Thiamine Hydrochloride RS in the Standard preparation; and RU and RS are the ratios of the peak areas of thiamine to methylbenzoate obtained from the Assay preparation and the Standard preparation, respectively.
Auxiliary Information— Please check for your question in the FAQs before contacting USP.
Topic/Question Contact Expert Committee
Monograph Huy T. Dinh, M.S.
Scientific Liaison
1-301-816-8594 (DS2010) Monographs - Dietary Supplements
Reference Standards RS Technical Services
1-301-816-8129
rstech@usp.org
USP34 – NF29 Page 4408
More
VOTE