Shen Yan, Han Chao, Liu Cuiping, Zhou Yongfang, Xia Biqi, Zhu Zhenou, Liu Aili
College of Chemistry and Materials Engineering, Wenzhou University, Wenzhou 325035, China
Se Pu. 2011 Feb;29(2):176-9. doi: 10.3724/sp.j.1123.2011.00176.
A method for the analysis of 4 alkaloids in Corydalis decumbens (Thunb.) Pers. was developed by high performance liquid chromatography-electrospray ionization tandem mass spectrometry (HPLC-MS/MS). The sample was extracted in methanol by ultrasonic, filtered and diluted with methanol for further analysis. The analysis was performed on a C18 column (150 mm x 2.1 mm, 3.5 microm) using a gradient elution program with the mobile phase of 0.2% acetic acid solution and acetonitrile. The analyte was determined by an electrospray ionization tandem mass spectrometry in multiple reactions monitoring (MRM) mode. The qualitative and quantitative analyses were based on the retention times and characteristic ion pairs consisting of one parent ion and two fragment ions of the analyte. The limits of detection (LODs) for 4 alkaloids were in the range of 0.02 - 0.2 microg/L, and the limits of quantification (LOQs) were in the range of 0.07 - 0.66 microg/L. The average recoveries were in the range of 93.6% - 103.5% for 4 alkaloids with the relative standard deviations below 3.8%. This method is reliable, sensitive and reproducible, and it can be used for the quality control of Corydalis decumbens (Thunb.) Pers. sample.
建立了一种采用高效液相色谱 - 电喷雾电离串联质谱法（HPLC-MS/MS）分析伏生紫堇中4种生物碱的方法。样品用甲醇超声提取，过滤后用甲醇稀释用于进一步分析。分析在C18柱（150 mm×2.1 mm，3.5微米）上进行，采用梯度洗脱程序，流动相为0.2%乙酸溶液和乙腈。通过电喷雾电离串联质谱在多反应监测（MRM）模式下测定分析物。定性和定量分析基于分析物的保留时间以及由一个母离子和两个碎片离子组成的特征离子对。4种生物碱的检测限（LOD）在0.02 - 0.2微克/升范围内，定量限（LOQ）在0.07 - 0.66微克/升范围内。4种生物碱的平均回收率在93.6% - 103.5%范围内，相对标准偏差低于3.8%。该方法可靠、灵敏且可重现，可用于伏生紫堇样品的质量控制。
