Institute of Legal Medicine, Hannover Medical School (MHH), Carl-Neuberg-Str. 1, D-30625 Hannover, Germany.
J Chromatogr B Analyt Technol Biomed Life Sci. 2019 May 1;1114-1115:1-4. doi: 10.1016/j.jchromb.2019.03.018. Epub 2019 Mar 18.
The ionisation of propofol was studied on the basis of analyte adduct formation with the components of the mobile phase. The identification of an appropriate propofol adduct ion generated in an acetate salt based buffer in the negative electrospray ionisation mode made the propofol LC-MS/MS analysis with two multiple reaction monitoring experiments possible without analyte derivatisation. Since a product ion of the deprotonated analyte was also used in the detection, these two fragmentation experiments were performed with different precursor ions. Liquid-liquid extraction with 1-chlorobutane was applied for sample preparation. A Luna 5 μm C18 (2) 100 A, 150 mm × 2 mm analytical column together with a mobile phase composed of water/methanol (3/97, v/v) with 10 mmol·L ammonium acetate and 0.1% acetic acid were applied. The limit of detection and quantification were 0.02 mg/L and 0.06 mg/L appropriate. Other results of the validation experiments performed like linearity of the calibration range, accuracy and precision, processed sample stability, recovery, matrix effect and selectivity revealed that this propofol quantification strategy developed can be defined as an applicable alternative to other methods presented.
基于与流动相成分形成分析物加合物的情况，研究了丙泊酚的电离。在乙酸盐缓冲液的负电喷雾电离模式下，生成合适的丙泊酚加合离子，从而实现了无需对分析物进行衍生化，即可通过两个多重反应监测实验进行丙泊酚 LC-MS/MS 分析。由于也使用了分析物去质子化的产物离子进行检测，因此这两个碎裂实验使用了不同的前体离子。采用 1-氯丁烷进行液-液萃取进行样品制备。使用 Luna 5μm C18（2）100A，150mm×2mm 分析柱，流动相由水/甲醇（3/97，v/v）组成，其中含有 10mmol·L 乙酸铵和 0.1%乙酸。检测限和定量限分别为 0.02mg/L 和 0.06mg/L。对其他验证实验结果进行了评估，如校准范围的线性、准确度和精密度、处理后样品稳定性、回收率、基质效应和选择性，结果表明，开发的这种丙泊酚定量策略可作为替代其他已报道方法的可行方法。
