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| 固相萃取-高效液相色谱法测定植物油中苯并\[a\]芘 |
| Determination of benzo\[a\] pyrene in vegetable oil by solid phase extraction and high performance liquid chromatography |
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| DOI：10.12166/j.zgyz.1003-7969/2020.03.010 |
| 中文关键词: 苯并\[a\]芘 固相萃取 高效液相色谱 植物油 |
| 英文关键词:benzo\[a\]pyrene solid phase extraction high performance liquid chromatography vegetable oil |
| 基金项目:大学生创新创业项目（201712709007） |
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| 中文摘要: |
| 建立了一种先用固相萃取法对样品进行前处理，再用高效液相色谱法测定苯并\[a\]芘含量的方法，同时研究了固相萃取柱的活化与重复使用。结果表明：苯并\[a\]芘标准曲线在0.5~10.0 μg/L范围内具有良好的线性关系，线性方程为y=60 267x+9 951（R2=0.999）；苯并\[a\]芘检出限为003 μg/kg，定量限为0.1 μg/kg，苯并\[a\]芘添加量在0.5~10.0 μg/kg的加标样品回收率均大于90%，变异系数小于5%。对6种不同食用油样品进行检测，本方法与国标法检测结果不存在显著差异（P>0.05）。固相萃取柱经乙酸乙酯简单的再活化处理后，可以重复使用。与国标法比较，本方法前处理步骤简单易操作、使用试剂量少、前处理时间短、检出限更低、方法回收率高，符合实验室和检测机构的检测需求。固相萃取柱可重复使用5次，可有效节约实验室的检测成本。 |
| 英文摘要: |
| A method for determination of benzo\[a\]pyrene using high performance liquid chromatography (HPLC) after a solid phase extraction sample pretreatment was established. The activation and reuse of solid phase extraction column were also studied at the same time. The results showed that the standard calibration curve of benzo\[a\]pyrene had a good linear relationship in the range of 0.5-10.0 μg/L with R2=0.999，the linear equation was y=60 267x+9 951. The detection limit of benzo\[a\]pyrene was 003 μg/kg and the quantitative limit was 0.1 μg/kg. The recovery of the spiked samples with dosage of benzo\[a\]pyrene 0.5-10.0 μg/kg was higher than 90% and the coefficient of variation was less than 5%. In the detection of six different edible oil samples, there was no significant difference between this method and the national standard method（P>0.05）. After a simple reactivation process using ethyl acetate, the extraction column could be reused. Compared with the national standard method, the pretreatment process of this method was simpler and easier to operate, the amount of reagents used was less, the pretreatment time was shorter, the detection limit was lower, and the recovery rate of the method was higher, which met the detection requirements of laboratories and testing organizations. Solid phase extraction column could be reused for five times, which could effectively save the testing cost of a laboratory. |
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