高效液相色谱法测定乳品中的纳他霉素残留

Determination of natamycin residue in milk products by high performance liquid chromatography

中文关键词:  乳品  纳他霉素  高效液相色谱法

英文关键词:milk products  natamycin  high performance liquid chromatography

中文摘要:

      目的 建立一种高效液相色谱法测定乳品中那他霉素残留的分析方法。方法 样品经提取、超声和离心分离后, 采用C18色谱柱(4.6 mm×250 mm, 5 μm)进行分离，高效液相色谱法测定。检测波长为302 nm, 流速为1.0 mL/min, 进样体积为10 μL, 柱温为30 ℃。对样品的提取溶剂和色谱流动相进行了优化, 并于国标测定方法的结果进行了比较。结果 选择10%的冰乙酸水溶液和0.1%的BHT-甲醇溶液作为样品提取溶剂, 甲醇-水-冰乙酸(60:40:6, V:V:V)作为流动相。本方法可以在7 min内完成对目标物的分离, 纳他霉素的标准曲线方程为Y=1.0058X+0.0715, 相关系数r=0.9995, 方法检出限为0.1 mg/kg。纳他霉素在3个添加水平下的回收率在96.8%~100%之间, 测定的相对标准偏差均小于1.18%。本方法与国标方法相比, 缩短了前处理时间, 提高了方法的回收率。结论 该方法快速、准确、精密度好, 适用于检测批量乳品中纳他霉素的残留量。

英文摘要:

      Objective To establish a method for the determination of natamycin residue in milk products by high performance liquid chromatography (HPLC). Methods After extraction, ultrasonic processing and centrifugal separation, the samples were detected by HPLC with C18 chromatographic column (4.6 mm×250 mm, 5 μm). The detection wavelength was 302 nm, the flow rate was 1.0 mL/min, the sample volume was 10 μL, and the column temperature was 30 ℃. Meanwhile, the extraction solvent of sample and chromatographic mobile phase were optimized, and the detection results were compared with that of standard method. Results The 10% glacial acetic acid aqueous solution and 0.1% BHT-methanol solution were selected as extraction solvent of sample, methanol-water-acetic acid (60:40:6, V:V:V) was selected as the chromatographic mobile phase. The separation of the target could be completed within 7 min. The standard curve equation of natamycin was Y=1.0058X+0.0715 (r=0.9995). Limit of detection of the method was 0.1 mg/kg. And the recoveries of natamycin at 3 spiked levels ranged from 96.8% to 100% with the relative standard deviation less than 1.18%. Compared with the national standard method, this method shorten the pretreatment time and increased the recovery. Conclusion The proposed method is fast, accurate and precise, which is suitable for the detecting of natamycin residue in numerous milk products.