Ohta H, Seto Y, Tsunoda N, Takahashi Y, Matsuura K, Ogasawara K
National Research Institute of Police Science, Tokyo, Japan.
J Chromatogr B Biomed Sci Appl. 1998 Sep 4;714(2):215-21. doi: 10.1016/s0378-4347(98)00241-2.
Determination of fourteen alkaloids, toxic Aconitum alkaloids, aconitine, mesaconitine, jesaconitine, hypaconitine and deoxyaconitine, and their hydrolysis products, benzoylaconines and aconines, have been established using capillary liquid chromatography (LC) fast atom bombardment mass spectrometry (FAB-MS) with a frit interface. Protonated molecular ions were observed as base peaks in the FAB-MS for these fourteen alkaloids. All the alkaloids were simultaneously quantified with linear gradient LC elution by solvent mixture of acetonitrile and 0.3% trifluoroacetic acid using selected ion monitoring of the protonated molecular ions. The calibration curves of these alkaloids were linear in injection amounts ranging from 5 to 500 pg, and their detection limits were 1 pg per injection (S/N=3). Solid-phase extraction using Sep-Pak Plus PS-1 was also investigated to clean-up and concentrate alkaloids in blood and urine samples, and showed satisfactory recoveries. This capillary LC-frit-FAB-MS method enables determination of low levels of Aconitum alkaloids in blood and urine samples, coupled with solid-phase extraction.
采用带烧结接口的毛细管液相色谱（LC）-快原子轰击质谱（FAB-MS）法，已实现对14种生物碱、有毒乌头生物碱、乌头碱、中乌头碱、次乌头碱、新乌头碱、去氧乌头碱及其水解产物苯甲酰乌头原碱和乌头原碱的测定。在FAB-MS中，这些14种生物碱的质子化分子离子被观测为基峰。使用乙腈和0.3%三氟乙酸的混合溶剂进行线性梯度LC洗脱，通过对质子化分子离子进行选择离子监测，对所有生物碱同时进行定量。这些生物碱的校准曲线在5至500 pg的进样量范围内呈线性，其检测限为每次进样1 pg（信噪比=3）。还研究了使用Sep-Pak Plus PS-1进行固相萃取，以净化和浓缩血液和尿液样本中的生物碱，并显示出令人满意的回收率。这种毛细管LC-烧结-FAB-MS方法结合固相萃取，能够测定血液和尿液样本中低水平的乌头生物碱。
