School of Pharmacy, Shenyang Pharmaceutical University, 103 Wenhua Road, Shenyang, 110016, PR China.
J Mass Spectrom. 2013 Jan;48(1):111-8. doi: 10.1002/jms.3133.
Chelidonium majus L. is one of the most important medicinal plants of the family Papaveraceae. Its pharmacological effects have been primarily attributed to the presence of a number of alkaloids. In the present study, a sensitive and selective liquid chromatography-tandem mass spectrometry method for simultaneous determination of five isoquinoline alkaloids from Chelidonium majus L. was developed and validated. The analytes (protopine, chelidonine, coptisine, sanguinarine and chelerythrine), together with the internal standard (palmatine), were extracted from acidified rat plasma with ethyl acetate-dichloromethane (4:1, v/v). Chromatographic separation was carried out on a Diamonsil C(18) column with an isocratic mobile phase consisting of acetonitrile and water (adjusted to pH 2.3 with formic acid) (30:70, v/v) at a flow rate of 0.4 ml/min. Mass spectrometric detection was performed by selected reaction monitoring mode via electrospray ionization source operating in positive ionization mode. The assay exhibited good linearity (r ≥ 0.9933) for all the analytes. The lower limits of quantification were 0.197-1.27 ng/ml using only 50 µl of plasma sample. The intra- and inter-day precisions were less than 11.9%, and the accuracy was between -6.3% and 9.3%. The method was successfully applied to the pharmacokinetic study of the five alkaloids in rats after intragastric administration of Chelidonium majus L. extract.
白屈菜是罂粟科最重要的药用植物之一。其药理作用主要归因于存在多种生物碱。本研究建立并验证了一种灵敏、选择性的同时测定白屈菜中 5 种异喹啉生物碱的液相色谱-串联质谱法。分析物（原阿片碱、白屈菜碱、小檗碱、血根碱和白屈菜红碱）和内标（巴马汀）经酸化大鼠血浆以乙酸乙酯-二氯甲烷（4:1，v/v）提取。采用 Diamonsil C(18)色谱柱，以乙腈和水（用甲酸调至 pH 2.3）（30:70，v/v）为流动相，流速为 0.4ml/min，进行等度洗脱分离。质谱检测采用电喷雾电离源，正离子模式下进行选择反应监测。所有分析物均表现出良好的线性（r≥0.9933）。采用仅 50μl 血浆样品，定量下限为 0.197-1.27ng/ml。日内和日间精密度均小于 11.9%，准确度在-6.3%至 9.3%之间。该方法成功应用于白屈菜提取物灌胃给药后大鼠 5 种生物碱的药代动力学研究。
