气相色谱法测定多酶片中残留溶剂含量  

Determination of residual solvents in multi-enzyme tablets by Gas chromatography

作　　者：周礼玲 张新芹 Zhou Liling;Zhang Xinqin(Lu'an Food and drug testing center,Lu'an,Anhui 237000,China;The integrated administrative enforcement detachment of the Lu'an Market Authority,Lu'an,Anhui 237000,China)

机构地区：[1]安徽省六安市食品药品检验中心,安徽六安237000 [2]安徽省六安市市场监管综合行政执法支队,安徽六安237000

出　　处：《首都食品与医药》2024年第10期174-176,共3页Capital Food Medicine

摘　　要：目的建立多酶片中两种残留溶剂的检测方法。方法采用顶空-气相色谱法,以DB-624毛细管柱(30m×0.53mm,3.0μm)为色谱柱,使用氢火焰离子化检测器(FID),载气为氮气,程序升温,初始温度40℃,维持8分钟,以每分钟10℃的速率升至100℃,维持1分钟,以每分钟20℃的速率升至220℃,维持7分钟;载气流速为每分钟2ml;进样口温度200℃;检测器温度250℃;顶空瓶平衡温度70℃,平衡30分钟。结果乙醇和丙酮可有效分离,检测限分别为0.5、0.1μg/ml,各溶剂线性关系良好,相关系数r均为1,乙醇回收率试验结果为96.8%,RSD为1.00%(n=6),丙酮回收率试验结果为103.6%,RSD为0.9%(n=6)。结论该方法操作简便、专属性强、准确度高,可应用于多酶片中残留溶剂的测定。Objective To establish a method for the determination of two residual solvents in multi-enzyme tablets.Methods Headspace Gas chromatography was used,DB-624 capillary column(30m×0.53mm,3.0μm)was used as chromatographic column,hydrogen flame ionization detector(FID)was used,carrier gas was nitrogen,temperature was programmed,initial temperature was 40℃,maintained for 8 minutes,at a rate of 10℃per minute to 100℃for 1 minute and at a rate of 20℃per minute to 220℃for 7 minutes,with a carrier gas flow rate of 2ml per minute,a sample inlet temperature of 200℃,a detector temperature of 250℃and a head-empty bottle equilibrium temperature of 70℃,balance for 30 minutes.Results Ethanol and acetone could be separated effectively.The detection limits were 0.5 and 0.1μg/ml,respectively.The Correlation Coefficient r was 1,the recovery rate of ethanol was 96.8%,RSD was 1.00%(n=6),the recovery rate of acetone was 103.6%.RSD was 0.9%(n=6).Conclusion The method is simple,specific and accurate for the determination of residual solvents in multi-enzyme tablets.

关 键 词：多酶片 气相色谱 残留溶剂 乙醇 丙酮 

分 类 号：R927.2[医药卫生—药学]