关闭
 
读者在线:用户名 密码
首页 期刊简介 投稿须知 期刊目录 专家风采 编委会 特邀顾问 联系我们 移动出版
  1. 1
  2. 2
  3. 3
  4. 4
  5. 5



刊物信息

期刊名称:药物分析杂志
主管单位:中国科学技术协会
主办单位:中国药学会
承办:中国食品药品检定研究院
主编:金少鸿
地址:北京天坛西里2号
邮政编码:100050
电话:010-67012819,67058427
电子邮箱:ywfx@nicpbp.org.cn
国际标准刊号:ISSN 0254-1793
国内统一刊号:CN 11-2224/R
邮发代号:2-237
 

访问统计
您是第  3 6 3 0 0 5 1 位浏览者
您当前的位置:首页 >> 正文

HPLC法测定间苯三酚中的基因毒性杂质2,4-二氯苯酚和2,4,6-三氯苯酚

Determination of genotoxic impurities of 2,4-dichlorophenol and 2,4,6-trichlorophenol in pyrogallol by HPLC

作者(英文):
分类号:R917
出版年·卷·期(页码):2018,38 (12):2110-2115
DOI: 10.16155/j.0254-1793.2017.01.01
-----摘要:-------------------------------------------------------------------------------------------

目的:建立一种高效液相色谱测定间苯三酚中的基因毒性杂质含量的方法。方法:采用Inertsil ODS-3 C18色谱柱(4.6 mm×250 mm,5 μm);流动相:以0.1%醋酸溶液为A相,乙腈为B相,进行梯度洗脱;流速:1.0 mL·min-1;检测波长:286 nm;柱温:35℃。结果:2,4-二氯苯酚和2,4,6-三氯苯酚回归方程分别为Y=1.742×104X+5.616(R2=0.999 7)和Y=1.399×104X-20.894(R2=0.999 5),其质量浓度在1.50~6.02 μg·mL-1和1.55~6.21μg·mL-1范围内与峰面积呈良好线性关系;定量下限分别为1.5和1.6 μg·mL-1;检测下限分别为0.5和0.5 μg·mL-1;平均回收率分别为99.5%(RSD=1.9%)和100.9%(RSD=1.4%)。3批样品中有2批检出2,4-二氯苯酚和2,4,6-三氯苯酚,其中含2,4-二氯苯酚分别为0.000 19%、0.000 18%,含2,4,6-三氯苯酚分别为0.000 22%、0.000 20%。结论:本法适用于间苯三酚中的基因毒性杂质检测及限度控制。

-----英文摘要:---------------------------------------------------------------------------------------

Objective: To establish an HPLC method for the determination of genotoxic impurities inpyrogallol.Methods: The method was achieved on an Intersil ODS-3 C18 column(4.6 mm×250 mm,5 μm). The mobile phase consisted of 0.1% acetic acid solution as mobile phase A and acetonitrile as mobile phase B with gradient elution at a flow rate of 1.0 mL·min-1.The detection wavelength was 286 nm and the column temperature was 35℃.Results: The concentration of 2,4-dichlorophenol in the range of 1.50-6.02 μg·mL-1 was in good linear relationship with the peak area.The regression equation was Y=1.742×104X +5.616(R2=0.999 7),and 2,4,6-trichlorophenol concentration in the range of 1.55-6.21 μg·mL-1 with the peak area was in good linear relationship,and the regression equation was Y=1.399×104X -20.894(R2=0.999 5). The quantification limits of 2,4-dichlorophenol and 2,4,6-trichlorophenol were 1.5 and 1.6 μg·mL-1,with the detection limits of 0.5 and 0.5 μg·mL-1,respectively. The average recoveries were 99.5%(RSD=1.9%) and 100.9%(RSD=1.4%),respectively.Sample measurement results show that the 2,4-dichlorophenol with content of 0.000 19% and 0.000 18%,and 2,4,6-trichlorophenol with content of 0.000 22% and 0.000 20% ware leteected in the two batches of samples,respectively.Conclusion: This method can be applicable to the detection and limit control of genotoxic impurities in pyrogallol.

-----参考文献:---------------------------------------------------------------------------------------

欢迎阅读《药物分析杂志》!您是该文第 244位读者!

药物分析杂志 © 2009
地址:北京天坛西里2号
邮政编码:100050; 技术支持:010-60213898

电子邮件:ywfx@nicpbp.org.cn