固相萃取-高效液相色谱法测定纸质食品包装材料中五氯酚含量

Determination of pentachlorophenol by solid phase extraction-high performance liquid chromatography in paper packaging materials for foodstuffs

中文关键词:  固相萃取  高效液相色谱法  纸质食品包装材料  五氯酚

英文关键词:solid phase extraction  high performance liquid chromatography  paper packaging materials for foodstuffs  pentachlorophenol

中文摘要:

      目的 建立固相萃取-高效液相色谱法测定纸质食品包装材料中五氯酚的分析方法。方法 2 g样品经过0.5%甲酸-甲醇超声提取2次, 合并提取液, 经Waters Oasis PRiME HLB (200 mg/6 mL)固相萃取小柱净化, 洗脱液氮吹浓缩至近干, 经甲醇复溶后采用高效液相色谱-二极管阵列检测器测定, 以C18柱为色谱柱, 甲醇-5 mmol/L乙酸铵(65:35, V:V)为流动相, 等度洗脱, 流速为1.0 mL/min, 柱温为35 ℃, 进样量为 20 μL, 检测波长为217 nm。结果 五氯酚在0.05~10.00 μg/mL范围内线性关系良好, 相关系数大于0.999, 检出限为0.01 mg/kg, 定量限为0.03 mg/kg, 平均加标回收率为84.7%~92.8%, 相对标准偏差(relative standard deviations, RSDs)为1.74%~4.79%。结论 该方法回收率高、重复性好、前处理简便, 可用于纸质食品包装材料中五氯酚的大批量检测。

英文摘要:

      Objective To establish an analytical method for the determination of pentachlorophenol in paper packaging materials for foodstuffs by solid phase extraction-high performance liquid chromatography. Methods The 2 g samples were ultrasonically extracted with 0.5% formic acid and methanol twice, the extracted solution was combined, and purified by Waters Oasis PRiME HLB (200 mg/6 mL) solid phase extraction cartridge, the eluent was concentrated by blowing nitrogen to near dryness, then redissolved in methanol, and determined by high performance liquid chromatography-diode array detector. The separation was performed on C18 column using methanol-5 mmol/L ammonium acetate (65:35, V:V) as mobile phase for isocratic elution. The flow rate was 1.0 mL/min, column temperature was 35 ℃, sample size was 20 μL, and the detection wavelength was 217 nm. Results Pentachlorophenol had a good linear relationship in the range of 0.05?10.00 μg/mL, the correlation coefficient was greater than 0.999, the limit of detection was 0.01 mg/kg, the limit of quantification was 0.03 mg/kg, and the average recoveries were 84.7%?92.8%, the relative standard deviations were 1.74%?4.79%. Conclusion The method has high recovery, good repeatability, simple pre-treatment, and can be used for large-scale detection of pentachlorophenol in paper packaging materials for foodstuffs.