菌渣中土霉素残留的高效液相检测法
霍 然1, 2,李再兴1, 2,钟为章1, 2,李贵霞
1. 河北科技大学 环境科学与工程学院,河北 石家庄 050018;2. 河北省污染防治生物技术实验室,河北 石家庄 050018
Determination of terramycin in terramycin bacterial residue by high performance liquid chromatography
Huo Ran1, 2, Li Zaixing1, 2, Zhong Weizhang1, 2, Li Guixia1, 2
1. School of Environmental Science and Engineering, Hebei University of Science and Technology, Shijiazhuang 050018,China; 2. Pollution Prevention Biotechnology Laboratory of Hebei Province, Shijiazhuang 050018, China
摘要 为准确检测土霉素菌渣中土霉素残留的含量,为土霉素菌渣无害化处理处置提供技术支撑,建立了一种菌渣中土霉素残留的高效液相色谱测定法。以甲醇+冰乙酸为提取剂,以甲醇+0.5%甲酸溶液为流动相、以C18柱为色谱柱,对样品进行检测。该方法在0.32~1000 mg·L-1线性范围内,线性相关系数为0.999 98,土霉素检出限(S / N = 3)为6.07 mg·kg-1。在0.4、1.2、2.0 mg·g-1添加水平下,回收率达到87.33% ~ 94.16%,相对标准偏差为5.46%,该方法定性定量准确,重现性好,可满足制药菌渣中土霉素残留检测的要求。
关键词 :
土霉素 ,
高效液相法 ,
土霉素菌渣
Abstract :To determine the concentration of terramycin in terramycin bacterial residue(TBR), and to provide technical references for the preliminary treatment and disposal of TBR, the determination method of terramycin residue amount in TBR by high performance liquid chromatography(HPLC) was established. First methanol and glacial acetic acid was used as extracting agent for pretreating the samples, then methanol and 0.1% formic acid aqueous solution was used as mobile phase, finally the C18 column was used as the chromatographic column for detection of terramycin. The linear range is 0.32 ~ 1 000 mg·L-1, the linear correlation coefficient is 0.999 98, and the method detection limit of terramycin(S/N=3) is 6.07 mg·kg-1. The recovery rate of each component is all 87.33% ~ 94.16% at three levels of 0.4, 1.2 and 2.0 mg·g-1, and the relative standard deviation is 5.46%. The method is accurate for qualitative and quantitative analysis, and has good reproducibility, and can satisfy the requirements of detecting terramycin residue in TBR.
Key words :
terramycin
high performance liquid chromatography
terramycin bacterial residue
基金资助: 河北省高等学校科学技术研究项目(QN2017332);河北省科技计划项目(17273806D);河北科技大学“五大平台开放基金课
题” (2018PT15)
通讯作者:
李贵霞,E-mail:lisun99@163.com
作者简介 : 霍 然( 1994— ),男,河北石家庄人,硕士研究生。
引用本文:
霍 然1, 2,李再兴1, 2,钟为章1, 2,李贵霞. 菌渣中土霉素残留的高效液相检测法[J]. 煤炭与化工, 2019, 42(12): 120-124.
Huo Ran1, 2, Li Zaixing1, 2, Zhong Weizhang1, 2, Li Guixia1, 2. Determination of terramycin in terramycin bacterial residue by high performance liquid chromatography. CCI, 2019, 42(12): 120-124.
链接本文:
http://www.mtyhg.com.cn/CN/10.19286/j.cnki.cci.2019.12.032 或 http://www.mtyhg.com.cn/CN/Y2019/V42/I12/120
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