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为了建立并验证一个液相色谱串联三重四级杆质谱法(LC-MS/MS)测定药材中的川楝素,供试品经甲醇水浴回流提取后,采用Agilent Eclipse Plus C18色谱柱(4.6 mm×100 mm,3.5μm),以乙腈-0.01%甲酸水溶液为流动相梯度洗脱,流速为0.5 mL/min,柱温30℃,进样量2μL.质谱条件为电喷雾电离源(ESI),负离子模式,选择离子监测(SIM),用于定量的离子为573.1.结果显示,川楝素在42.73~2 136.40 ng/mL范围内线性关系良好(R2=0.999 6),加样回收率为99.34%~106.53%,日内、日间精密度(RSD)均低于3%,最低检出限(LOD)为0.92 mg/kg,最低定量限(LOQ)为3.05 mg/kg,稳定性较好.说明所建方法能够高效快捷地对川楝素进行测定,且方法简便、专属性强、灵敏度高,测定结果准确可靠,适用于川楝子、苦楝皮中川楝素的定性定量测定,也为其新制剂的设计和开发提供方法参考.
To establish and validate a LC-MS / MS method for the determination of toosendanin in medicinal materials, the samples were extracted with a methanol-water bath and extracted with an Agilent Eclipse Plus C18 column (4.6 mm × 100 mm, 3.5 μm) with a mobile phase of acetonitrile-0.01% formic acid as mobile phase at a flow rate of 0.5 mL / min and a column temperature of 30 ° C. The injection volume was 2 μL.The mass spectrometry conditions were electrospray ionization source (ESI) Negative ion mode, ion selective detection (SIM), the ion used for quantification was 573.1.The results showed that toosendanin was good linearity (R2 = 0.999 6) in the range of 42.73 ~ 2 136.40 ng / mL with the recovery of 99.34 % ~ 106.53%. The RSD was less than 3%, the minimum detectable limit (LOD) was 0.92 mg / kg, the lowest limit of quantification (LOQ) was 3.05 mg / kg and the stability was good. The results showed that the proposed method could be used to determine toosendanin efficiently and quickly. The method was simple, specific, sensitive and accurate. The method was suitable for the qualitative and quantitative determination of toosendanin in Toona sinensis and Melia azedarach, Design and development of new formulations provide a method reference.