GC法测定不同级别乳酸中残留溶剂的含量  

Determination of Residual Solvents in Different Grades of Lactic Acid by GC Method

作　　者：张悦 赵勇 郑金凤 刘雁鸣 谢莹莹 ZHANG Yue;ZHAO Yong;ZHENG Jin-feng;LIU Yan-ming;XIE Ying-ying(Hunan Institute for Drug Control(Hunan Center for Pharmaceutical Excipients Control),Changsha 410001,China;Hunan Engineering&Technology Research Center for Pharmaceutical Quality Evaluation,Changsha 410001,China)

机构地区：[1]湖南省药品检验研究院(湖南药用辅料检验检测中心),湖南长沙410001 [2]湖南省药品质量评价工程技术研究中心,湖南长沙410001

出　　处：《海峡药学》2022年第8期54-57,共4页Strait Pharmaceutical Journal

摘　　要：目的建立GC法测定乳酸中甲醇、乙醇含量的方法,为乳酸质量控制提供依据。方法采用气相色谱法,DB-624毛细管柱(30 m×0.32 mm,1.8μm),程序升温:起始温度为40℃,维持5 min,以20℃/min的速率升温至200℃/min,维持4 min;进样口温度为250℃;FID检测器温度为250℃;分流比:10∶1;顶空瓶平衡温度:90℃;平衡时间:30 min;柱流量(N _(2)):2 mL·min^(-1)。结果在实验条件下,各残留溶剂之间能完全分离;甲醇、乙醇在0~150μg·mL^(-1)的浓度范围线性关系良好(r ^(2)≥0.9997),平均回收率分别为91.14%(RSD:2.67%)、88.20%(RSD:3.04%)。结论本方法准确度高、重现性好,可用于乳酸中残留溶剂的测定。OBJECTIVE Establish a GC method to determine the content of methanol and ethanol in lactic acid to provide a basis for the quality control of lactic acid.METHODS Using gas chromatography,DB-624 capillary column(30 m×0.32 mm,1.8μm),program temperature rise:the initial temperature 40℃,maintain for 5 minutes,and the temperature was increased to 200℃at a rate of 20℃per minute,maintain for 4 minutes;inlet temperature 250℃,FID detector temperature 250℃,split ratio 10∶1,equilibrium temperature 90℃,equilibrium time 30 min,column flow rate(N _(2)):2 mL·min^(-1).RESULTS Under the chromatographic condition,the residual solvents can be completely separated;the linear relationship of methanol and ethanol in the concentration range of 0-150μg·mL^(-1)were good(r≥0.9997),and the average recovery rates were 91.14%(RSD:2.67%)and 88.20%(RSD:3.04%),respectively.CONCLUSION The method has high accuracy and good reproducibility,and can be used for the determination of residual solvents in lactic acid.

关 键 词：乳酸 甲醇 乙醇 残留溶剂 气相色谱法 

分 类 号：R927[医药卫生—药学]