摘要
提出了高效液相色谱-串联质谱法测定葛根中葛根素和大豆苷元的含量。样品经乙醇提取,所得提取液用乙醇定容至100mL后经Waters Xterra MS C18色谱柱(150mm×3.9mm,5μm)分离,用乙腈与50mmol.L-1甲酸溶液(40+60)的混合液洗脱,采用电喷雾正离子电离多反应监测模式。葛根素和大豆苷元的质量浓度分别在0.050~0.50mg.L-1和5.0~50mg.L-1之间与峰面积呈线性关系,检出限(3S/N)均为5μg.L-1。在0.1,1.0,10.0mg.L-1 3个浓度水平进行加标回收试验,葛根素和大豆苷元的回收率分别为96.6%和97.4%。
HPLC-MS/MS was applied to the determination of pueratin and daidzein in puerarin root. The sample was extracted with ethanol, and the extract obtained was filtrated, made up to 100 mL with ethanol and used for HPLC-MS/MS determination, using Waters Xterra MS C18 column (150 mm×3. 9 mm, 5 μm) as chromatographic column, and a mixture of acetonitrile and 50 mmol·L^-1 ammonium acetate solution (mixed in the ratio of 40 to 60 by vol. ) as mobile phase. Positive electrospray ionization and multiple reaction monitoring mode were used in the detection. Linear relationships between values of peak area and mass concentration were obtained in ranges of 0. 050--0. 50 mg·L^-1 (for pueratin) and 5.0--50 mg·L^-1 (for daidzein), with same detection limits (3S/N) of 5μg ·L^-1 Tests for recovery were performed by standard addition method at 3 concentration levels of 0. 1,1.0, 10. 0 mg·L^-1 ; results of recovery of pueratin and daidzein found were 96.6% and 97.4% respectively.
出处
《理化检验(化学分册)》
CAS
CSCD
北大核心
2013年第4期464-467,共4页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)