摘要
目的:建立疏风活络丸中伪麻黄碱、麻黄碱、士的宁和马钱子碱含量的GC-MS测定方法。方法:采用Variancp-sil 8 CB Low bleed/MS毛细管柱(30m×250μm,0.25μm)分离,升温程序:起始温度50℃,保持1min,以25℃/min升至135℃,保持6min,以30℃/min升至300℃,保持22min。进样口温度为280℃;载气为He,恒流方式,柱流量为1mL/min,不分流进样1μL。MS采用EI离子源,离子源温度230℃;电子能量70 eV,传输管温度300℃,全扫描方式采集定性,质量范围40～450m/z;伪麻黄碱、麻黄碱采用总离子定量,士的宁和马钱子碱采用选择离子定量。结果:4种生物碱达到良好分离。方法平均回收率分别为伪麻黄碱97.82%(RSD2.70%)、麻黄碱98.76%(RSD3.23%)、士的宁98.00%(RSD2.18%)和马钱子碱98.19%(RSD1.89%)(n=6)。结论:所建立的方法可靠,能准确测定疏风活络丸中4种生物碱类的含量。
Aim： To develop a GC-MS method for the determination of pseudoephedrine, ephedrine, strychnine and brucine in Shufeng Huoluo pills. Methods： Chromatographic separation of these four alkaloids was carried out on the capillary column （ Varian cp-sil 8 CB Low bleed/MS （ 30 m × 250 μm, 0. 25 μm） ）, using helium as carrier gas at a constant flow rate of 1 mL/min. The column oven was subject to the temperature program beginning from 50℃ in 1 min, rising to 135 ℃ at a rate of 25 ℃/min, and standing for 6 min before reaching 300 ℃ at a rate of 30 ℃/min and remained for 22 min. Inlet temperature was set at 280 ℃, and 1μL was injected in a splitless mode in all cases. Mass spectrometer was operated in electron impact （El） mode at an electron energy of 70 eV. The ion source was set at 230 ℃, and the transfer line 300 ℃. The quantitation was conducted in full-scan mode with the range of 40-450 m/z. Total ions were used to calculate the amounts of pseudoephedrine, and ephedrine; and the selected ions were selected to quantitate those of strychnine and brucine. Results： There existed excellent chromatographic separation of the four species. The estimated recoveries for pseudoephedrine, ephedrine, strychnine and brucine were 97.82% （ RSD 2. 70%）, 98.76% （ RSD 3.23%）, 98.00% （ RSD 2. 18%）, and 98.19% （ RSD 1.89%）, respectively. Conclusion： The established method .is accurate, reliable, and practicable in the determination of the four alkaloids in Shufeng Huoluo pills.
出处
《中国药科大学学报》
CAS
CSCD
北大核心
2008年第6期519-522,共4页
Journal of China Pharmaceutical University
