摘要
目的建立一种基于固相萃取-高效液相色谱串联四级杆飞行时间质谱检测人全血中马钱子碱的检测方法。方法样品过Oasis HLB固相萃取小柱,经3 m L去离子水淋洗,有机溶剂洗脱后,在Zorbox Eclipse Plus C18（2.1mm×50mm,1.8μm）色谱柱上分离,以0.1%甲酸水溶液-甲醇为流动相梯度洗脱,流速为0.3 m L/min,四级杆飞行时间串联质谱检测。通过计算500 ng/m L马钱子碱对照样品在上述固相萃取和色谱质谱条件下,不同洗脱溶剂以及不同洗脱体积下的回收效率从而优化洗脱溶剂的种类和使用量。结果以甲醇为洗脱溶剂,加入量为3 m L时,马钱子碱在200-2000 ng/m L的添加水平下回收率为80.1%-101.3%,相对标准偏差为5.2%-8.3%。人全血中马钱子碱在50-5000 ng/m L范围内线性良好（R^2=0.999 97）,检测限为10.2 ng/m L,最低定量限为34.1 ng/m L。结论该方法快速方便,回收率和灵敏度高,可用于人全血中马钱子碱的定量测定。
Objective To develop a simple method for determination of brucine in the whole blood based on solid phase extraction （SPE） and high-performance liquid chromatography/electrospray ionization with quadrupole time-of-flight tandem mass spectrometry （HPLC/QTOF-MS）. Methods The samples were extracted in HLB column with 3 mL water and organic solvent to be separate as the washing and elution solvent. The extracts were analyzed with Zorbox Eclipse Plus C 18 （2.1 mm×50 mm, 1.8μm） column and gradient elntion by mobile phase consisted of water （containing 0.1% formic acid）-methanol at 0.3 mL/min, and the involvement of quadrupole time of flight tandem MS detector. The type and volume of elution were optimized by calculation of recovery efficiency of 500 ng/mL brucine of the control sample subjected to the different elution solvent and volume. Results Under the optimal condition of 3 mL elution solvent of methanol, the recovery rate of brucine in the blood at 200-2000 ng/mL level was 80.1%-101.3%, and the corresponding standard deviations （ RSDs, n=3） 5.2%-8.3%. The calibration curves were linear over 50 -5000 ng/mL （R^2=0.99997）, the limit of detection （LOD） 10.2 ng/ mL, and the limit of quantity （LOQ） 34.1 ng/mL. Conclusions The method is simple, accurate and convenient for qualitative and quantitative determination of brucine in the human whole blood.
出处
《刑事技术》
2015年第5期417-419,共3页
Forensic Science and Technology
