高效液相色谱法测定2-(4-硝基苯基)丁酸有关物质  

Determination of Related Substances of 2-(4-Nitrophenyl) Butanoic Acid by High Performance Liquid Chromatography

作　　者：孙孝丽 姜明明 杜国辉[2] 李素敏 周娟 孙迎基 李铁军 SUN Xiao-li;JIANG Ming-ming;DU Guo-hui;LI Su-min;ZHOU Juan;SUN Ying-ji;LI Tie-jun(Shandong Jingwei Pharmaceutical Co.,Ltd.,Tai’an 271000,China;Shandong Institute of Commerce and Technology,Jinan 250000,China)

机构地区：[1]山东京卫制药有限公司,山东泰安271000 [2]山东商业职业技术学院,山东济南250000

出　　处：《食品与药品》2024年第6期557-560,共4页Food and Drug

摘　　要：目的建立2-(4-硝基苯基)丁酸中有关物质的高效液相色谱(HPLC)检测方法。方法用十八烷基硅烷键合硅胶为填充剂[推荐使用Agilent Infinity Lab Poroshell 120 EC-C_(18)(4.6 mm×250 mm,4μm)或效能相当的色谱柱];以水(用磷酸调节pH值至2.5)-乙腈(90:10)为流动相A,以水-乙腈(10:90)为流动相B,梯度洗脱;流速为1.0 ml/min;柱温为30℃;检测波长为215 nm;进样体积10μl。结果2-(4-硝基苯基)丁酸及其10个杂质在一定的范围内线性关系良好;杂质i-8与2-(4-硝基苯基)丁酸的分离度大于1.2,其他各成分峰之间的分离度均大于1.5;各成分的检出限在0.02~0.07μg/ml内;精密度试验中各杂质含量回收率RSD均不高于6%;各杂质的回收率均在92.17%~106.40%范围内;供试品溶液室温条件下放置27.5 h内有关物质没有明显变化;更换色谱柱、改变柱温、流速、流动相的pH和流动相的初始比例,有关物质的检测结果无明显变化。结论该方法专属性强,灵敏度高,可用于2-(4-硝基苯基)丁酸中有关物质的检测。Objective To establish a high performance liquid chromatography(HPLC)method for the detection of related substances in 2-(4-nitrophenyl)butyric acid.Methods Octadecylsilane bonded silica gel was used as filler[Agilent Infinity Lab Poroshell 120 EC-C_(18)(4.6 mm×250 mm,4μm)was recommended,or chromatographic column with equivalent efficiency],using water(adjusted to pH 2.5 with phosphoric acid)-acetonitrile(90:10)as mobile phase A and water-acetonitrile(10:90)as mobile phase B for gradient elution.The flow rate was 1.0 ml/min,the column temperature was 30℃,the detection wavelength was set at 215 nm,and the injection volume was 10μl.Results The linearity of 2-(4-nitrophenyl)butyric acid and its 10 impurities was good within certain linear ranges.The resolution between 2-(4-nitrophenyl) butyric acid and impurity i-8 was greater than 1.2, and the resolution between the peaks of other components was greater than 1.5. The detection limit of each component was 0.02-0.07 μg/ml. The RSDs of the recoveries of all the impurities in the precision test were not higher than 6 %. The recoveries of all impurities were within the range of 92.17 %-106.40 %. There was no significant changes in the contents of the relevant substances within 27.5 h at room temperature. Replacing the chromatographic column, changing the column temperature, flow rate, pH of the mobile phase, and initial ratio of the mobile phase did not result in significant changes in the detection results of the relevant substances. Conclusion This method has strong specificity and high sensitivity, and it can be used for the detection of related substances of 2-(4-nitrophenyl) butyric acid.

关 键 词：2-(4-硝基苯基)丁酸 高效液相色谱 有关物质 

分 类 号：R927[医药卫生—药学]