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[求助]
GC样品分析问题，谢谢大家了。。
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药典方法求助 各位老师，帮帮忙。以下是药典方法： Silylation solution. To 2 mL of N,O-bis(trimethylsilyl)tri- fluoroacetamide R add 0.04 mL of chlorotrimethylsilane R and mix. Test solution.Dissolve50.0mgofthesubstancetobeexamined in 3 mL of water R and add 0.5 mL of hydrochloric acid R. Extract with 2 quantities, each of 5 mL, of methylenechlorideR. Evaporate the combined methylene chloride extracts to dryness in a vial with a screw cap and add 0.5 mL of the silylation solution.Sealthevialandheatat70±5°Cfor20min. 其中，Seal the vial and heat at 70±5°C for 20min.这个是单单指硅烷化反应的温度和时间吗？有没有包括后面顶空平衡的温度和时间？还是说后面顶空平衡的温度和时间需要自己摸索设定? |
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ltxin2009
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4楼2012-02-07 16:17:25
ltxin2009
铁杆木虫 (职业作家)
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2楼2012-02-07 12:00:46
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这是整个气相方法： TESTS pH (2.2.3): 6.5 to 7.5. Dissolve 0.20 g in carbon dioxide-free water R and dilute to 10 mL with the same solvent. Impurity C. Gas chromatography (2.2.28). Silylation solution. To 2 mL of N,O-bis(trimethylsilyl)tri- fluoroacetamide R add 0.04 mL of chlorotrimethylsilane R and mix. Test solution.Dissolve50.0mgofthesubstancetobeexamined in 3 mL of water R and add 0.5 mL of hydrochloric acid R. Extract with 2 quantities, each of 5 mL, of methylenechlorideR. Evaporate the combined methylene chloride extracts to dryness in a vial with a screw cap and add 0.5 mL of the silylation solution.Sealthevialandheatat70±5°Cfor20min. Reference solution (a).Dissolve5.0mgof sodium phenylbutyrate impurity C CRS in methylenechlorideR and dilute to 10.0 mL with the same solvent. Reference solution (b). Dilute 1.0 mL of reference solution (a) to 10.0 mL with methylenechlorideR.Place1.0mLofthis solution in a vial with a screw cap, evaporate to dryness and add 0.5 mL of the silylation solution. Seal the vial and heat at 70±5°Cfor20min. Reference solution (c). Dissolve 10 mg of the substance to be examined in 25 mL of water R. To 3 mL of this solution add 0.1 mL of hydrochloric acid R. Extract with 2 quantities, each of 5 mL, of methylene chloride R. Combine the methylene chloride extracts in a vial with a screw cap and add 2 mL of reference solution (a). Evaporate to dryness and add 0.5 mL of the silylation solution. Seal the vial and heat at 70 ± 5 °C for 20 min. Column: — material :fusedsilica; — size: l =25m,Ø=0.25mm; — stationary phase: poly(dimethyl)(diphenyl)siloxane R (film thickness 1.0 μm). Carrier gas : helium for chromatography R. Flow rate:0.9mL/min. Split ratio: 1:100. Temperature: Time(min) Temperature(°C) Column 0-5 50 5 - 27 50 → 270 27 – 32 270 Injection port 270 Detector 270 Detection:flameionisation. Injection:1 μL. Relative retention with reference to phenylbutyrate (retention time = about 20 min) : impurity C = about 0.98. System suitability: reference solution (c) : — resolution: minimum 3.0 between the peaks due to impurity C and phenylbutyrate. Limit : — impurity C:notmorethantheareaofthecorresponding peak in the chromatogram obtained with reference solution (b) (0.1 per cent). Related substances. Liquid chromatography (2.2.29). |
3楼2012-02-07 16:07:41
