固相萃取-气相色谱-质谱法测定3种中药材中18种多环芳烃

建立了固相萃取-气相色谱-质谱法测定3种中药材中18种多环芳烃(PAHs)的检测方法. 选取丹参、平贝母、厚朴为样品基质, 以正己烷提取, 经Fiorisil、ProElut PAH专用固相萃取柱联合净化. 采用DM-PAH柱分离, 选择离子监测(SIM)模式检测, 基质匹配外标法定量. 结果表明: 实际样品中, 18种PAHs在5 ~200 μg/L的质量浓度内线性关系良好, 相关系数均大于0.998. 检出限在0.6~1.2 μg/kg之间, 定量限在2.0~4.0 μg/kg之间. 以4.0、8.0、40.0 μg/kg添加水平进行方法学验证, 丹参的回收率为81.5%~106.3%, 相对标准偏差在1.5%~7.8%之间. 平贝母的回收率为87.1%~108.3%, 相对标准偏差在2.1%~8.4%之间. 厚朴的回收率为82.4%~107.9%, 相对标准偏差在1.8%~6.9%之间. 方法净化效率高, 准确度、灵敏度良好, 可用于丹参、平贝母和厚朴3种中药材样品中18种PAHs类化合物的检测.

Determination of Eighteen Polycyclic Aromatic Hydrocarbons in Three Traditional Chinese Medicine Herbs by Solid Phase Extraction-Gas Chromatography-Mass Spectrometry

A simple and rapid method for the determination of 18 polycyclic aromatic hydrocarbons (PAHs) in 3 traditional Chinese medicine (TCM) herbs has been established using the solid phase extraction-gas chromatography-mass spectrometry (SPE-GC-MS). Salvia miltiorrhiza, Fritillaria ussuriensis and Magnolia officinalis were selected as the samples. The samples were extracted with n-hexane. The extracts were purified on Florisil cartridges and Proelut-PAH SPE columns. 18 PAHs were separated on DM-PAH columns (30 m×0.25 mm×0.25 μm). Selective ion monitoring (SIM) mode was used for the mass spectrometry, and matrix-matched external standard method was used for the quantification. The results showed that the 18 PAHs had a good linearity over the concentration range of 5~200 μg/L and the correlation coefficients (R2) were all greater than 0.998. The limit of detections (LODs) were 0.6~1.2 μg/kg (S/N=3) and the limit of quantifications (LOQs) were 2.0~4.0 μg/kg(S/N=10). The recoveries (spiked at 4.0, 8.0, 40.0 μg/kg) were 81.5%~106.3% (Salvia miltiorrhiza), 87.1%~108.3% (Fritillaria ussuriensis) and 82.4%~107.9% (Magnolia officinalis), respectively. The relative standard deviations (RSDs) were 1.5%~7.8% (Salvia miltiorrhiza), 2.1%~8.4% (Fritillaria ussuriensis) and 1.8%~6.9% (Magnolia officinalis), respectively. The method has a high purification efficiency, accuracy and sensitivity, and can be used for the detection of 18 PAHs in TCM herbs. Using this method, Salvia miltiorrhiza, Fritillaria ussuriensis and Magnolia officinalis samples were tested and found to have varied levels of PAHs. This method can provide theoretical and practical significance for the detection of PAHs in TCM herbs.