LIU Hongmin, HUANG Lei, LIAO Xuandong, ZHAO Wensong, LI Shuhua, LI Shaopeng, FANG Ping, LIU Qingqing, LIU Shuai, LI Hong
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Objective To detect the chloroephedrine by ultra-performance liquid chromatography in tandem with mass spectrum (UPLC-MS/MS). Methods UPLC-MS/MS was conducted with the mobile phase that was consisted of acetonitrile and 0.3% formic acid in water, running in gradient elution, along with mass spectrometric acquisition being carried out by electrospray ionization in positive mode (ESI+) plus multiple reaction monitoring (MRM). Multiple characteristic ion pairs (184.2/148.2, 184.2/91.2 and 184.2/133.2) and retention time were adopted to chloroephedrine for qualitative analysis, and the external standard method was used for quantitative analysis. In comparison of the solubility and stability of chloroephedrine in 9 kinds of common extraction solvents, the chloroform was shown the best. Results For chloroephedrine, its linear range was 1~100 ng/mL, linear equation: A = 45000×C + 49700, and the linear relationship being well with the correlation coefficient as 0.9993, the qualitative and quantitative restriction showing 0.01 ng/mL and 0.04 ng/mL, respectively. The precision was less than 10% and the accuracy higher than 90%. Conclusion This method is of higher sensitivity and good accuracy for chloroephedrine detection, with chloroform the best solvent.