UHPLC-MS/MS法测定天麻胶囊中6种生物碱含量
Determination of Six Alkaloids in Tianma Capsule by UHPLC-MS/MS
王娟娟 1谭春梅 1张晨辉 1陈碧莲 1方翠芬1
作者信息
- 1. 浙江省食品药品检验研究院,国家药品监督管理局中成药质量评价重点实验室,杭州 310052
- 折叠
摘要
目的 建立超高效液相色谱串联质谱(UHPLC-MS/MS)法同时测定天麻胶囊中苯甲酰新乌头原碱、苯甲酰乌头原碱、苯甲酰次乌头原碱、新乌头碱、次乌头碱和乌头碱6种生物碱的含量.方法 采用Phienomenex Kinetex C18色谱柱(2.1 mm ×100 mm,2.6 μm);流动相为甲醇和体积分数0.1％甲酸水(含2.5 mmol·L-1乙酸铵)溶液,梯度洗脱,流速为0.3 mL·min-1,柱温为35 ℃;采用电喷雾离子源,以多反应离子监测模式进行质谱检测.结果 苯甲酰新乌头原碱、苯甲酰乌头原碱、苯甲酰次乌头原碱、新乌头碱、次乌头碱和乌头碱分别在 79.38～3 969 ng·mL-1(r=0.999 9)、18.60～929.8 ng·mL-1(r=0.999 8)、38.20～1 910 ng·mL-1(r=0.999 9)、1.264～252.8 ng·mL-1(r=0.999 3)、1.196～239.2 ng·mL-1(r=1.000 0)和 1.268～253.6 ng·mL-1(r=1.000 0)内有良好的线性关系.重复性试验结果,各化合物含量RSD为0.5％～3.2％,平均回收率为98.3％～105.3％,RSD为1.0％～3.4％.结论 该方法专属性好,灵敏度高,准确可靠耐用,可用于天麻胶囊中6种生物碱的含量测定.
Abstract
OBJECTIVE To establish an UHPLC-MS/MS method for the determination of six alkaloids in Tianma capsule.METHODS Phenomenex Kinetex C18(2.1 mm × 100 mm,2.6 μm)column was used for separation.The mobile phase consisted of methanol and 0.1％formic acid(containing 2.5 mmol·L-1 ammonium acetate)solution(gradient elution).The flow rate was 0.3 mL·min-1 and the column temperature was maintained at 35 ℃.Electrospray positive ion source was used for mass spectrometry detection by multiple reaction monitoring mode.RESULTS The liner range of calibration curve was 79.38-3 969 ng·mL-1(r=0.999 9),18.60-929.8 ng·mL-1(r=0.999 8),38.20-1 910 ng·mL-1(r=0.999 9),1.264-252.8 ng·mL-1(r=0.999 3),1.196-239.2 ng·mL-1(r=1.000 0)and 1.268-253.6 ng·mL-1(r=1.000 0)for benzoylmesaconine,benzoy-laconine,benzoylhypaconine,mesaconitine,hypaconitine and aconitine.The RSD of repeatability test(content)was 0.5％-3.2％.The average recoveries was in the range of 98.3％-105.3％.RSD was 1.0％-3.4％.CONCLUSION The method has good sprcificity,sensitivity and accuracy,and it is suitable for the analysis of six alkaloids in Tianma capsule.
关键词
天麻胶囊/附子/生物碱/超高效液相色谱串联质谱法/含量测定Key words
Tianma capsule/Aconiti Lateralis Radix Praeparata/alkaloid/UHPLC-MS/MS/assay引用本文复制引用
出版年
2024
NETL
NSTL
万方数据