2种测定抗菌药物水分方法的比较研究

Comparison of Two Methods for Determination of Antibiotic Moisture

关键词:  抗菌药物  水分  气相色谱法  费休氏法

Key words:  antibiotics  water  gas chromatography(GC)  Fisher's method

摘要:

目的 采用气相色谱法和费休氏法测定抗菌药物中水分的含量，探讨使用气相色谱法测定抗菌药物水分含量的可行性。方法 气相色谱法采用顶空毛细管气相色谱-热导检测器法进行测定，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。费休氏法采用中国药典2015年版四部通则0832中水分测定第一法中的容量滴定法。结果 除了注射用头孢曲松钠和注射用头孢唑肟钠外，其他抗菌药物样品2种测定方法测定结果无显著性差异。结论 本研究所建立的气相色谱法，可用于部分抗菌药物水分含量的测定。

Abstract:

OBJECTIVE Determination of water content in antibiotics by gas chromatography and Fisher's method, to investigate the feasibility of determination of water content in antibiotics by gas chromatography. METHODS Determination by gas chromatography with a headspace capillary gas chromatography-thermal conductivity detector method by using Agilent HP-PLOT/Q(30 m×0.530 mm, file 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℃, keep 6 min, 60℃ per minute at a rate of up to 250℃, keep 5 min. The detector temperature of thermal conductivity detector was 250℃ and the current was 70 mA. Fisher's method adopted the volumetric titration method in the first method of moisture determination in the fourth general rule 0832 of the 2015 edition of the "People's Republic of China Pharmacopoeia". RESULTS Except ceftriaxone sodium for injection and cefazoloxime sodium for injection, there was no significant difference between the two determination methods for other antibiotic samples. CONCLUSION The gas chromatography established in this paper can be used to determine the moisture content of some antibiotics.