目的建立地黄中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0.1~2.0 ng/mL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1µg/kg,在1、5、10μg/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,适用于中药材生、熟地黄中3,4-苯并(a)芘的快速检测。% Objective To develop a method for the rapid determination of 3,4-benzo(a)pyrene in Reh-manniae. 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 (HPLC) with fluorescence detector. Results The method showed a good linearity over the range of 0.1~2.0 ng/mL for 3,4-benzo(a)pyrene with R=0.999. LOQ was 1μg/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 suitable for the rapid analysis of 3,4-benzo(a)pyrene in Rehmanniae..
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