加速溶剂萃取-气相色谱-三重四极杆串联质谱法测定地黄中苯并芘

Determination and confirmation of benzopyrene in Chinese herbal medicines Rehmanniae Radix and Rehmanniae Radix Praeparata by gas chromatography- triple quadrupole tandem mass spectrometry

目的：建立中药材地黄中苯并芘的加速溶剂萃取-气相色谱-三重四极杆串联质谱（GC-QQQ-MS/MS）分析方法，并对10个地黄样品进行苯并芘残留测定。方法：以中性氧化铝为填料，乙腈为萃取剂，加速溶剂萃取法（ASE）对地黄样品进行提取和净化，提取液浓缩后，采用GC-QQQ-MS/MS技术在多反应监测模式（MRM）下测定，外标法定量。结果：苯并芘进样浓度在10~200 ng·mL-1范围内呈良好线性（相关系数0.991），苯并芘在3个添加水平下（2、5和10 μg·kg-1）回收率为82.0%~96.5%，重复性RSD（n=6）为7.4%~17.8%，方法精密度RSD（n=6）为5.7%，检出限（LOD）1 ng·kg-1，定量限（LOQ）2 ng·kg-1。结论：方法灵敏度满足国内外苯并芘限量要求，并可进行定性确证用于中药材致癌污染物苯并芘监测。

Objective： To develop an analysis method based on gas chromatography-triple quadrupole tandem mass spectrometry （GC-QQQ-MS/MS） with accelerated solvent extraction （ASE） for the determination and qualitative confirmation of benzopyrene in Rehmanniae Radix and Rehmanniae Radix Praeparata,and to quantify benzopyrene in 10 samples. Methods： Benzopyrene in the test samples was extracted and purified by ASE with neutral alumina as filler and acetonitrile as solvent.The prepared samples were analysed by GC-QQQ-MS/MS in multiple reaction monitoring （MRM） modes,and an external standard method was applied to quantify benzopyrene. Results： The calibration curves showed good linear relationship between the area and the concentration of benzopyrene from 10 to 200 ng·mL-1 with a correlation coefficient of 0.991.The average recoveries of benzopyrene ranged from 82.0% to 96.5% at three spiked levels of 2,5 and 10 μg·kg-1.The repeatability RSD（n=6） was in the range of 7.4% to 17.8%.The precision RSD （n=6） of the instrument was 5.7%,the limit of detection （LOD） was 1 ng·kg-1 and the limit of quantity （LOQ） was 2 ng·kg-1. Conclusion： Sensitivity of this method meets the requirements of domestic and foreign benzopyrene residue limits and the qualitative confirmation can be achieved.