动态显色法检测谷氨酸中细菌内毒素含量  

Determination of Bacterial Endotoxin in Glutamic Acid by Kinetic Chromogenic Assay

作　　者：王冲 徐军田 王祖璇 侯娟 华晓东 WANG Chong;XU Juntian;WANG Zuxuan;HOU Juan;HUA Xiaodong(Tianjin Institute for Drug Control,Tianjin 300070,China)

机构地区：[1]天津市药品检验研究院,天津300070

出　　处：《中国药学杂志》2025年第3期302-307,共6页Chinese Pharmaceutical Journal

摘　　要：目的建立定量检测谷氨酸中细菌内毒素的方法,并验证其可行性。方法依据《中国药典》2020年版通则1143细菌内毒素检查法中动态显色法的标准,采用两个厂家的鲎试剂,通过细菌内毒素标准曲线的可靠性验证实验、供试品前处理中所用试剂钙离子缓冲液及磷酸氢铵钠的干扰实验、供试品的干扰实验及外加内毒素回收实验,成功建立了谷氨酸中细菌内毒素的检测方法,并对3批供试品进行了定量检测。结果将供试品与磷酸氢铵钠一起溶解,配制成质量浓度为20mg·mL^(-1)的谷氨酸溶液,以钙离子缓冲液稀释至5mg·mL^(-1)以下,对细菌内毒素检查无干扰作用。3批供试品的内毒素含量均小于限值12EU·g^(-1),相对标准偏差(RSD)均<10%,阳性回收率在50%~200%,符合规定。结论本研究所建立的细菌内毒素检查方法可用于谷氨酸的细菌内毒素检查,控制其产品质量。OBJECTIVE To establish a method for the quantitative detection of bacterial endotoxin in glutamic acid and verify its feasibility.METHODS Verification test of the reliability of bacterial endotoxin standard curve,interference test of calcium ion buffer and sodium ammonium hydrogen phosphate used in pre-treatment,and interference test of test product and additional endotoxin recovery test were carried out in sequence by using limulus reagents from two manufacturers according to the standard of kinetic chromogenic assay in bacterial endotoxin inspection method(General Chapter 1143 in Chinese Pharmacopoeia2020 Edition).A method for the detection of bacterial endotoxin in glutamic acid was successfully established,and three batches of samples were quantitatively detected by this method.RESULTS Glutamic acid was dissolved with sodium ammonium hydrogen phosphate together to the concentration of 20 mg·mL^(-1),then diluted by calcium ion buffer to the concentration of 5 mg·mL^(-1),which had no interference effects on bacterial endotoxin test.The contents of endotoxin in three batches of samples were all lower than the limit of 12 EU·g^(-1),the RSD values were all lower than 10%,and the endotoxin recovery rates were in the range of 50%to 200%,which met the requirements.CONCLUSION The bacterial endotoxin test method established in this study can be used to detect the bacterial endotoxin in glutamic acid and control its quality.

关 键 词：谷氨酸 原料药 细菌内毒素 动态显色法 定量检测 

分 类 号：R917[医药卫生—药物分析学]