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高效液相色谱与QDA质谱联用同时测定附子理中丸中6个单酯及双酯型生物碱含量 被引量:1

Simultaneous determination of six diterpenoid alkaloids in Fuzilizhong pills by HPLC coupled with QDA mass detector
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摘要 目的:建立同时测定附子理中丸中6个单酯及双酯型生物碱含量的方法。方法:应用高效液相色谱(HPLC)与QDA质谱联用同时测定附子理中丸中苯甲酰新乌头原碱、苯甲酰次乌头原碱、苯甲酰乌头原碱、新乌头碱、次乌头碱和乌头碱6个成分的含量。使用Phenomenex Luna C_(18)色谱柱(4.6 mm×250 mm,5μm),以乙腈-0.2%乙酸水(用三乙胺调p H 6.2)为流动相,梯度洗脱,流速1.0 m L·min~(-1),分流比为1∶4,使用ESI~+离子源,选择性离子扫描(SIM)模式下对苯甲酰新乌头原碱(m/z 590.0)、苯甲酰乌头原碱(m/z 604.0)、苯甲酰次乌头原碱(m/z 574.0)、新乌头碱(m/z 632.0)、次乌头碱(m/z 616.0)和乌头碱(m/z 646.0)进行测定。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、次乌头碱、新乌头碱和乌头碱6个成分的质量浓度分别在0.000 2~51.75μg·m L~(-1)(r=0.999 2)、0.000 2~50.95μg·m L~(-1)(r=0.999 5)、0.000 2~50.25μg·m L~(-1)(r=0.999 8)、0.000 2~49.80μg·m L~(-1)(r=0.999 9)、0.000 2~50.60μg·m L~(-1)(r=0.999 5)和0.000 2~52.00μg·m L~(-1)(r=0.999 7)范围内线性关系良好;平均回收率(n=6)分别为101.8%、101.3%、98.2%、104.8%、99.9%和89.9%,RSD分别为6.4%、2.6%、2.7%、6.1%、3.8%和5.7%。3批附子理中丸中6个生物碱成分即苯甲酰新乌头原碱、苯甲酰次乌头原碱、苯甲酰乌头原碱、新乌头碱、次乌头碱和乌头碱的含量范围分别为7.095~7.366、1.007~1.214、0.594~0.742、1.261~1.438、1.492~1.578和0.135~0.163μg·g~(-1)。结论:该方法可测定附子理中丸中6个生物碱成分含量,为附子理中丸的质量标准提高打下了基础。 Objective:To establish the quantitative method of six diterpenoid alkaloids in Fuzilizhong pills.Methods:The contents of benzoylmesaconitine,benzoylaconitine,benzoylhypaconitine,mesaconitine,aconitine,and hypaconitine in Fuzilizhong pills were determined by HPLC coupled with QDA mass detector.The chromatographic column was Phenomenex Luna C_(18)(4.6 mm×250 mm,5μm).The mobile phase was the mixture of acetonitrile-0.2%acetic acid(adjust p H to 6.2 with triethylamine)in gradient mode,the flow rate was1.0 m L·min~(-1),and the split ratio was 1∶4.The ESI~+source of the mass spectrometer was used in selected ion monitoring(SIM)mode for the detection of benzoylmesaconitine(m/z 590.0),benzoylaconitine(m/z 604.0),benzoylhypaconitine(m/z 574.0),mesaconitine(m/z 632.0),aconitine(m/z 646.0)and hypaconitine(m/z616.0).Results:The linear ranges of benzoylmesaconitine,benzoylaconitine,benzoylhypaconitine,hypaconitine,mesaconitine,and aconitine were 0.000 2-51.75μg·m L~(-1)(r=0.999 2),0.000 2-50.95μg·m L~(-1)(r=0.999 5),0.000 2-50.25μg·m L~(-1)(r=0.999 8),0.000 2-49.80μg·m L~(-1)(r=0.999 9),0.000 2-50.60μg·m L~(-1)(r=0.999 5)and 0.000 2-52.00μg·m L~(-1)(r=0.999 7),respectively.The average recovery rates(n=6)of the above compounds were 101.8%,101.3%,98.2%,104.8%,99.9%and 89.9%with RSD of 6.4%,2.6%,2.7%,6.1%,3.8%and5.7%,respectively.The contents of benzoylmesaconitine,benzoylhypaconitine,benzoylaconitine,mesaconitine,aconitine and hypaconitine were 7.095-7.366,1.007-1.214,0.594-0.742,1.261-1.438,1.492-1.578 and 0.135-0.163μg·g~(-1),respectively.Conclusion:The method can be used to determine the content of six diterpenoid alkaloids in Fuzilizhong pills.The present study provides a scientific basis for the quality control of Fuzilizhong pills.
作者 张聿梅 何轶 李耀磊 周超 于健东 戴忠 马双成 ZHANG Yu-mei1, HE Yi1, LI Yao-lei1, ZHOU Chao2, YU Jian-dong1, DAI Zhong1, MA Shuang-cheng1( 1. National Institutes for Food and Drug Control, Beijing 100050, China; 2. Qiqihaer Food and Drug Inspection Control, Qiqihar 161000, China )
出处 《药物分析杂志》 CSCD 北大核心 2018年第7期1248-1253,共6页 Chinese Journal of Pharmaceutical Analysis
关键词 附子理中丸 单酯型生物碱 双酯型生物碱 苯甲酰新乌头原碱 苯甲酰次乌头原碱 苯甲酰乌头原碱 新乌头碱 次乌头碱 乌头碱 液相色谱-质谱联用 QDA质谱 含量测定 Fuzilizhong pills monoester alkaloid diester alkaloid benzoylmesaconitine benzoylaconitine benzoylhypaconitine mesaconitine aconitine hypaconitine LC-MS QDA mass spectrometer quantitative determination
作者简介 Tel:(010)67095994;E—mail:zhangyumei@nicpbp,org.cn;通信作者于健东Tel:(010)67095896;E-mail:yujiandong@nicpbp.org.cn;通信作者马双成Tel:(010)67095272;E-mail:msc@nicpbp.org.cn
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