加速溶剂萃取-液相色谱法快速测定中药材地黄中 3, 4-苯并(a)芘残留

Rapid determination of 3,4-benzo(a)pyrene in Chinese herbal medicines Rehmanniae by accelerated solvent extraction and HPLC with fluorescence detector

中文关键词:  3,4-苯并(a)芘  地黄  高压液相色谱法  加速溶剂萃取

英文关键词:3,4-benzo(a)pyrene  rehmannia  high pressure liquid chromatography  accelerated solvent extraction

中文摘要:

      的 建立地黄中 3,4-苯并(a)芘的高压液相色谱快速测定方法。 方法 地黄样品用乙腈作提取剂经加速溶剂萃取, 中性氧化铝净化除去吸附杂质和色素后采用高压液相色谱-荧光检测法快速测定。 结果 3,4-苯并(a)芘在 1~20 ?g/kg 含量范围内线性关系良好, 线性方程为 Y=8.66e3X 4.11 e3, 相关系数为 0.999。本方法的定量限为 1 ?g/kg, 在 1、 5、 10 μg/kg 三个加标水平下, 加标回收率为 87.0%~93.1%, 相对标准偏差为 7.7%~14.3% (n=6)。结论 该方法简便快速、灵敏可靠, 适用于原地黄中中药材生、熟地黄中 3,4-苯并(a)芘的快速检测。

英文摘要:

      Objective A method was developed for the rapid determination of 3,4-benzo(a)pyrene in Rehmanniae. Methods Samples were extracted with acetonitrile through accelerated solvent extraction (ASE) with neutral alumina as filler, purified by neutral alumina to eliminate the great mass of coextracts such as pigments and impurity, and then detected by high pressure liquid chromatography with fluorescence detector. Results The method showed a good linearity over the range of 1～20 μg/kg for 3,4-benzo(a)pyrene with R=0.999. LOQ was 1 μg/kg. The recoveries were 87.0%~93.1% at the spiked level of 1, 5, and 10 μg/kg with relative standard deviation of 7.7%~14.3% (n=6). Conclusion This method is simple and accurate, and it is suitable for the rapid analysis of 3,4-benzo(a)pyrene in Rehmanniae..