摘要
目的 建立癃闭康泰中贝母素甲、贝母素乙的高效液相色谱-质谱联用含量测定法。方法 癃闭康秦片经碱化，用氯仿-甲醇（4：1）提取生物碱有效部位，提取液浓缩，残渣用甲醇溶解后，进行高效液相色谱-质谱测定。色谱柱为Agilent Zorbax extend C18（2．1mm×100mm，5μm）；流动相为乙腈和10mmol·L^-1甲酸铵（pH8．0），梯度洗脱（0．15min：乙腈30％．55％；15．25min乙腈55％）；流速0．2mL·min^-1；柱温30℃。质谱条件为电喷雾电离源（ESI），以选择性正离子方式检测，贝母素甲和贝母素乙的选择性检测离子分别为m／z432．4和m／z430．4。结果 贝母素甲和贝母素乙的的线性范围均为0．01．10mg·L^-1，相关系数均大于0．999，检测限均为0．45μg·L^-1，方法回收率均大于95％，日内日间精密度（RSD）均小于5％。结论 本方法专属性强，灵敏度高，线性关系良好，操作简便，适用于癃闭康泰中贝母素甲、贝母素乙的含量测定。
OBJECTIVE To develop a sensitive and specific LG-MS method for the determination of peimine and peiminine in Longbikangtain tablet.METHODS The drug was extracted with a mixed solution of chloroform-methanol（4：1） after being alkalined.The LC-MS method was performed on a Agilent Zorbax Extend-C18（2.1 mm×150 mm,5μm） .The mobile phase consisted of CH3CN and 10 mmoL·L^-1 ammonium formate （pH 8.0） at a gradient elution.The flow rate was at 0.2 mL＂ min- l .The temperature of column was 30℃. Esi was applied and operated in positive mode.The monitor ions were m/z 432.4（peimine） and m/z 430.4（peiminine）. RESULTS The linear calibration curve of peimine and peiminine were observed in the concentration range of 0.01 - 10 mg·L^-1 .The lower limit of quantification of peimine and peiminine were 0.45 μg·L^-1. The relative recoveries were more than 95 %. The inter-and intraday precision （RSDS） were below 5.0%. CONCLUSION The method is proved to be convenient, sensitive and rapid, and suitable for the determination of peimine and peiminine in Longbikangtain tablet.
出处
《中国药学杂志》
CAS
CSCD
北大核心
2006年第13期1026-1028,共3页
Chinese Pharmaceutical Journal
作者简介
俞滢，女，讲师
通讯作者：朱亚尔，女，副教授 Tel：（0571）86971871 E-mail：zhuyaer@zju．edu．cn
