【求助】USP 硬脂富马酸钠 薄层色谱法检查杂质
发布于 2013-10-21 · 浏览 5173 · IP 重庆重庆
这个帖子发布于 11 年零 197 天前，其中的信息可能已发生改变或有所发展。
各位战友，有谁按照USP检查过硬脂富马酸钠的杂质的，标准原文如下：
Solvent: Chloroform andglacial acetic acid (4:1)
Standard monostearyl maleatestock solution: 1 mg/mL of USP Monostearyl Maleate RS in Solvent
Standard monostearyl maleatesolution: Pipet 5.0 mL of Standard monostearyl maleate stock solution,and dilute with chloroform to 50 mL.
Standard stearyl alcohol stocksolution: 1 mg/mL of USP Stearyl Alcohol RS in Solvent
Standard stearyl alcoholsolution: Pipet 5.0 mL of Standard stearyl alcohol stock solution,and dilute with chloroform to 50 mL.
Sample solution: Transfer200 mg of Sodium Stearyl Fumarate to a small, glass-stoppered conical flask.Add 10.0 mL of Solvent. Dissolve by placing the flask in an ultrasonicbath for 10 min.
Chromatographic system
(See Chromatography 621 , Thin-Layer Chromatography.)
Mode: TLC
Adsorbent: 0.25-mm layerof chromatographic silica gel (TLC plates)
Spray reagent: Sulfuricacid and alcohol (1:9). [Note— Addcautiously and with stirring. ]
Developing solventsystem: Hexanes, toluene, and glacial acetic acid (5:5:1)
Analysis
Samples: Standardmonostearyl maleate solution, Standard stearyl alcohol solution, and Samplesolution
Apply 5 ?L of Standardmonostearyl maleate solution and 10 ?L each of Standard stearyl alcoholsolution and Sample solution to the plate. Immerse the plate in atank containing a layer of 10 mm of chloroform on the bottom. Allow the solventfront to reach the upper edge of the spots. Withdraw the plate, and dry in acurrent of cold air. Repeat the immersion, development, and drying. Thisresults in spots having a linear shape. Develop the chromatograph in asaturated chamber containing the Developing solvent system until thesolvent front has moved 15 cm, and remove the plate from the chamber. Allow todry for 10 min, and heat in an oven at 90for 2 min. Allow to cool to room temperature. Replace the plate in the chamberfor another 15-cm development, remove the plate, and allow to dry at roomtemperature for 15 min. Spray the plate with Spray reagent. Dry theplate in an oven at 150for 15 min. Dark spots appear on a light background. Allow to cool. Faint spotsat an R F value of 0.9 may result from traces ofdistearyl maleate and distearyl fumarate.
Acceptance criteria: Theintensity of any spot from the Sample solution is not greater than thatfrom the corresponding spot from the Standard monostearyl maleate solutionand Standard stearyl alcohol solution (NMT 0.25% sodium stearyl maleate,NMT 0.5% stearyl alcohol).
请教各位战友，Faint spots at an R F value of 0.9 may result from traces of distearyl maleate and distearyl fumarate.这句话，以及最后的Acceptance criteria这一整段话应该怎么理解。
我做出来的图见附件，做了好几次都是一样的
Solvent: Chloroform andglacial acetic acid (4:1)
Standard monostearyl maleatestock solution: 1 mg/mL of USP Monostearyl Maleate RS in Solvent
Standard monostearyl maleatesolution: Pipet 5.0 mL of Standard monostearyl maleate stock solution,and dilute with chloroform to 50 mL.
Standard stearyl alcohol stocksolution: 1 mg/mL of USP Stearyl Alcohol RS in Solvent
Standard stearyl alcoholsolution: Pipet 5.0 mL of Standard stearyl alcohol stock solution,and dilute with chloroform to 50 mL.
Sample solution: Transfer200 mg of Sodium Stearyl Fumarate to a small, glass-stoppered conical flask.Add 10.0 mL of Solvent. Dissolve by placing the flask in an ultrasonicbath for 10 min.
Chromatographic system
(See Chromatography 621 , Thin-Layer Chromatography.)
Mode: TLC
Adsorbent: 0.25-mm layerof chromatographic silica gel (TLC plates)
Spray reagent: Sulfuricacid and alcohol (1:9). [Note— Addcautiously and with stirring. ]
Developing solventsystem: Hexanes, toluene, and glacial acetic acid (5:5:1)
Analysis
Samples: Standardmonostearyl maleate solution, Standard stearyl alcohol solution, and Samplesolution
Apply 5 ?L of Standardmonostearyl maleate solution and 10 ?L each of Standard stearyl alcoholsolution and Sample solution to the plate. Immerse the plate in atank containing a layer of 10 mm of chloroform on the bottom. Allow the solventfront to reach the upper edge of the spots. Withdraw the plate, and dry in acurrent of cold air. Repeat the immersion, development, and drying. Thisresults in spots having a linear shape. Develop the chromatograph in asaturated chamber containing the Developing solvent system until thesolvent front has moved 15 cm, and remove the plate from the chamber. Allow todry for 10 min, and heat in an oven at 90for 2 min. Allow to cool to room temperature. Replace the plate in the chamberfor another 15-cm development, remove the plate, and allow to dry at roomtemperature for 15 min. Spray the plate with Spray reagent. Dry theplate in an oven at 150for 15 min. Dark spots appear on a light background. Allow to cool. Faint spotsat an R F value of 0.9 may result from traces ofdistearyl maleate and distearyl fumarate.
Acceptance criteria: Theintensity of any spot from the Sample solution is not greater than thatfrom the corresponding spot from the Standard monostearyl maleate solutionand Standard stearyl alcohol solution (NMT 0.25% sodium stearyl maleate,NMT 0.5% stearyl alcohol).
请教各位战友，Faint spots at an R F value of 0.9 may result from traces of distearyl maleate and distearyl fumarate.这句话，以及最后的Acceptance criteria这一整段话应该怎么理解。
我做出来的图见附件，做了好几次都是一样的
最后编辑于 2022-10-09 · 浏览 5173
6 收藏点赞
