气相色谱-质谱法测定食品用纸制品中五氯酚含量

Determination of pentachlorophenol by gas chromatography mass spectrometry in paper packaging materials for foodstuffs

中文关键词:  五氯酚  食品用纸制品  衍生  内标法  气相色谱-质谱法

英文关键词:pentachlorophenol  paper packaging materials for foodstuffs  derivatization  internal standard method  gas chromatography mass spectrometry

中文摘要:

      目的 建立气相色谱-质谱法测定食品用纸制品中五氯酚含量的分析方法, 了解食品用纸制品中五氯酚的残留状况。方法 纸制品试样加入2,4,6-三溴酚内标后, 经液-液萃取, SLC柱净化, 乙酸酐-吡啶溶液衍生后, 采用气相色谱-质谱法测定, 内标法定量。结果 在50～1000 ng范围内, 相关系数均>0.9995。方法的检出限为0.008 mg/kg, 定量限为0.025 mg/kg。加标回收率为89.3%~109.8%, 相对标准偏差(relative standard deviations, RSDs)分别为3.2%、8.6%和4.4%。106份市售纸制品中, 8份样品检出五氯酚, 阳性率为7.5 %, 含量范围为0.011~0.045 mg/kg, 阳性样品五氯酚含量的平均值为0.027 mg/kg。结论 该方法灵敏度较高, 精密度好, 适用于纸制品中五氯酚的准确定量检测。检测数据表明, 食品用纸制品中五氯酚风险较小。

英文摘要:

      Objective To establish an analytical method for the determination of pentachlorophenol in food paper products by gas chromatography-mass spectrometry. Methods After adding 2,4,6-tribromophenol internal standard to paper products, the samples were extracted by liquid-liquid extraction, purified by SLC column, and derivatized by acetic anhydride pyridine solution. The samples were determined by gas chromatography-mass spectrometry, and quantified by internal standard method. Results The correlation coefficients were over 0.9995 in the range of 50?1000 ng. The limit of detection was 0.008 mg/kg and the limit of quantification was 0.025 mg/kg. The recoveries were 89.3%?109.8%, and the relative standard deviations (RSDs) were 3.2%, 8.6% and 4.4%, respectively. Pentachlorophenol was detected in 8 samples of 106 paper products, and the positive rate was 7.5%. The content range was 0.011?0.045 mg/kg, and the average content of pentachlorophenol was 0.027 mg/kg. Conclusion The method has high sensitivity and good precision, and is suitable for the accurate quantification of pentachlorophenol in paper products. The test data showed that the risk of pentachlorophenol in food paper products was low.