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yzhlasiI鐵蟲 (正式寫手)
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[求助]
GC樣品分析問題，謝謝大家了。。
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藥典方法求助 各位老師，幫幫忙。以下是藥典方法： 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.這個(gè)是單單指硅烷化反應(yīng)的溫度和時(shí)間嗎？有沒有包括后面頂空平衡的溫度和時(shí)間？還是說后面頂空平衡的溫度和時(shí)間需要自己摸索設(shè)定? |
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yzhlasiI
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這是整個(gè)氣相方法： 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). |
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