高效液相色谱法检测牛奶中的氟哌啶醇残留

Determination of haloperidol in milk by high performance liquid chromatography

中文关键词:  高效液相色谱法  氟哌啶醇  牛奶  外标法

英文关键词:high performance liquid chromatography  haloperidol  milk  external standard method

中文摘要:

      目的 建立高效液相色谱法检测牛奶中氟哌啶醇残留量的分析方法。方法 样品采用酸化乙腈(0.2%甲酸, V:V)提取, C18固相萃取小柱净化, 氮吹浓缩后, 经0.45 μm滤膜过滤, 使用安捷伦ZORBAX SB-C18色谱柱进行分离, 乙腈-0.2%甲酸水溶液(1:1, V:V)作为流动相以0.3 mL/min流速等度洗脱, 外标法定量。结果 经选择, 紫外检测波长为254 nm, 此条件下, 氟哌啶醇质量浓度(X, μg/mL)与其峰面积(Y)在0.2~5.0 μg/mL范围内, 线性关系良好, 相关系数为0.999, 在3.0、7.0、10.0 μg/mL 3水平的加标回收率为81.73%~95.57%, 相对标准偏差为1.97%, 检出限为7.58 μg/L, 定量限为25.27 μg/L。结论 此方法具有成本低、操作简单、可操作性强、回收率高、灵敏度高、精确度高等优点, 适用于牛奶中氟哌啶醇的检测。

英文摘要:

      Objective To establish a method for the determination of haloperidol residues in milk by high performance liquid chromatography. Methods The samples was extracted with acidified acetonitrile (0.2% formic acid, V:V), purified by C18 solid phase extraction column, concentrated by nitrogen blowing, filtered by 0.45 μm filter membrane, separated by Agilent ZORBAX SB-C18 column with the acetonitrile-0.2% formic acid aqueous solution (1:1, V:V) as mobile phase and isometric elution was performed at 0.3 mL/min, and quantified by external standard method. Results The selected ultraviolet detection wavelength was 254 nm, under this condition, the linear relationship between haloperidol concentration (X, μg/mL) and peak area (Y) was good in the range of 0.2?5.0 μg/mL, the correlation coefficient was 0.999, and the spiked recoveries at 3.0, 7.0, 10.0 μg/mL were 81.73%?95.57%, the relative standard deviation was 1.97%, the limit of detection was 7.58 μg/L, and limit of quantification was 25.27 μg/L. Conclusion This method has the advantages of low cost, simple operation, strong operability, high recovery, high sensitivity and high accuracy, which is suitable for the detection of haloperidol in milk.