气相色谱水分测定法的改进研究

目的：改进《中华人民共和国药典》2015年版四部通则0832气相色谱水分测定的方法，并初步探讨用本法取代费休氏法用于测定抗生素中水分的可行性。方法：采用顶空毛细管气相色谱-热导检测器法，使用Agilent HP-PLOT/Q毛细管色谱柱（30 m×0.530 mm×40 μm），载气为高纯氦气，流量3 mL·min^-1，进样量250 μL，分流比20：1，进样口温度为200℃；柱升温程序：初始温度150℃，保持6 min，以60℃·min^-1的速率升到250℃，保持5 min；热导检测器温度为250℃，电流为70 mA进行测定。结果：改进的气相色谱法方法学验证成立，且操作简便、准确、可靠，克服了《中华人民共和国药典》方法的不足，可用于药品中水分的质量控制。结论：本法可取代费休氏法用于部分抗生素的水分测定，与《中华人民共和国药典》2015年版四部通则0832中水分测定的第五法（气相色谱法）相比具有一定的优越性。

Objective: To improve the method of water content determination by gas chromatography in the Volume IV of the China Pharmacopoeia 2015,and to discuss the feasibility of the method instead of Fischer's method for the determination of water content in antibiotics. Methods: A headspace capillary gas chromatography-thermal conductivity detector (HCGC-TCD) method was established for the determination by using Agilent HP-PLOT/Q (30 m×0.530 mm×40 μm) capillary column. The high purity helium was used as the carrier gas with the flow of 3 mL·min^-1. The injection volume was 250 μL with the split ratio of 20:1. The injection temperature was 200℃. The column temperature program:initial temperature 150℃,keeping for 6 min,then raise up to 250℃ at a rate of 60℃·min^-1,keeping for 5 min.The detector temperature of thermal conductivity detector (TCD) was 250℃ and the current was 70 mA. Results: The improved gas chromatography method has been validated,and the operation was simple,accurate,and reliable. It overcomes the lack of Pharmacopoeia methods and can be used for the quality control of water content in drugs. Conclusion: This method can replace the Fisher's method for water content determination in some antibiotics,and has certain advantages over the gas chromatography for water content determination in the general chapters of the ChP 2015.

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