气相色谱-质谱法测定水产品中的10种含氯苯酚及其盐类的含量

Determination of ten chlorinated phenols and their salts in aquatic products by gas chromatography-mass spectrometry

中文关键词:  三氯苯酚  四氯苯酚  五氯苯酚  水产品  鱼  虾  气相色谱-质谱法

英文关键词:trichlorophenol  tetrachlorophenol  pentachlorophenol  aquatic products  fish  shrimp  gas chromatography- mass spectrometry

中文摘要:

      目的 建立气相色谱-质谱法检测水产品中10种含氯苯酚的含量。方法 样品采用1mol/L氢氧化钾溶液超声提取, 经乙酸酐衍生, 用正己烷提取后采用气相色谱-质谱法(gas chromatography-mass spectrometry, GC-MS)进行检测, 以外标法定量。结果 10种含氯苯酚在2.0~50.0 ?g/L浓度范围内具有良好的线性关系, 相关系数r大于0.999, 方法定量限为2.5 μg/kg。空白基质加标回收实验添加浓度分别为2.5、12.5和62.5 ?g/kg时, 水产品中10种含氯苯酚的回收率在85.1%~104.5%之间, 相对标准偏差≤5.0%。结论 该方法灵敏度、精密度和定量限均符合实际样品检测要求, 可用于水产品中含氯苯酚及其盐类的日常监测。

英文摘要:

      Objective To establish a method for the determination of 10 kinds of chlorinated phenols in aquatic products by gas chromatography-mass spectrometry(GC-MS). Methods Using ultrasonic extraction, samples were extracted with 1mol/L KOH solution, derivatized with acetic anhydride, and extracted with n-hexane,and then analyzed by gas chromatography-mass spectrometry(GC-MS) with external standard method for quantification. Result Ten kinds of chlorinated phenols had good linear relationshipin the range of 2.0~50.0 ?g/Lwith correlation coefficient not less than 0.999. And the limit of quantitation (LOQ) was 2.5 μg/kg.The recoveries spike at 3 levels of 2.5, 12.5 and62.5 ?g/kg were ranged from 85.1% to 104.5 using blank samples as matrix with relative standard deviations (RSD) less than or equal to 5.0%. Conclusion The sensitivity, precision and LOQ can meet the requirements of determination of practical samples, which can be applied for the regular inspection of chlorinated phenols and their salts in aquatic products.