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

作　　者：王娟娟 谭春梅 张晨辉 陈碧莲 方翠芬 WANG Juanjuan;TAN Chunmei;ZHANG Chenhui;CHEN Bilian;FANG Cuifen(NMPA Key Laboratory for Quality Evaluation of Traditional Chinese Medicine,Zhejiang Institute for Food and Drug Control,Hangzhou 310052,China)

机构地区：[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

出　　处：《中国药学杂志》2024年第22期2179-2186,共8页Chinese Pharmaceutical Journal

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Phenomenex Kinetex C_(18)色谱柱(2.1 mm×100 mm,2.6μm);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79.38~3969 ng·mL^(-1)(r=0.9999)、18.60~929.8 ng·mL^(-1)(r=0.9998)、38.20~1910 ng·mL^(-1)(r=0.9999)、1.264~252.8 ng·mL^(-1)(r=0.9993)、1.196~239.2 ng·mL^(-1)(r=1.0000)和1.268~253.6 ng·mL^(-1)(r=1.0000)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。OBJECTIVE To establish an UHPLC-MS/MS method for the determination of six alkaloids in Tianma capsule.METHODS Phenomenex Kinetex C_(18)(2.1 mm×100 mm,2.6μm)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 79.38-3969 ng·mL^(-1)(r=0.9999),18.60-929.8 ng·mL^(-1)(r=0.9998),38.20-1910 ng·mL^(-1)(r=0.9999),1.264-252.8 ng·mL^(-1)(r=0.9993),1.196-239.2 ng·mL^(-1)(r=1.0000)and 1.268-253.6 ng·mL^(-1)(r=1.0000)for benzoylmesaconine,benzoylaconine,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 

分 类 号：R917[医药卫生—药物分析学]