摘要
本文建立了一种使用岛津超高效液相色谱仪Nexera X2和三重四极杆质谱仪LCMS-8050联用测定水蛭配方颗粒中7种碱基和核苷成分的分析方法.水蛭配方颗粒以10%甲醇50℃超声提取30 min,MRM正负模式同时检测.以Discovery■HS F5-3色谱柱进行分离,流动相为0.15%甲酸水溶液和甲醇,10 min内完成梯度洗脱.本方法采用外标法定量,7种化合物在相应的浓度范围内线性关系良好,判定系数(R^(2))均大于0.996,定量限在0.42—3.94μg·g^(-1)之间. 10 ng·mL^(-1)的混合标准品溶液连续进样6次,待测化合物峰面积RSD均小于6%,精密度良好.平行6份加标回收试验,7种化合物平均回收率在87.09%—105.81%之间,RSD%在1.35%—4.70%之间.残留实验结果为阴性.该方法准确可靠,可为水蛭配方颗粒的质量控制提供参考依据.
An analytical method was established for simultaneous determination of 7 nucleobase and nucleoside components in leech formula granule by a combination of Shimadzu ultra-high performance liquid chromatography Nexera X2 and triple quadrupole mass spectrometry LCMS-8050.Leech formula granule was extracted by ultrasound at 50℃with 10%methanol for 30 minutes,and detected with MRM mode by both positive and negative ESI ionization.Discovery®HS F5-3 column was used for separation,with a mobile phase consisted of 0.15%formic acid aqueous solution and methanol.Gradient elution was used within 10 minutes.External standard method was used for quantification.The seven compounds had good linear relationships within the corresponding concentration range,all coefficient of determination(R^(2))were greater than 0.996,and the quantification limit was between 0.42μg·g^(-1)and 3.94μg·g^(-1).The 10 ng·mL^(-1) mixed standard solution was injected 6 times,and the peak area RSD of tested compounds was all less than 6%,indicating good precision.The recovery experiments executed for six times,the average recovery of 7 compounds was ranged from 87.09%to 105.81%,with RSD%ranging from 1.35%to 4.70%.The residual test result was negative.This method is accurate and reliable,and can provide a reference for the quality control of leech formula granule.
作者
姜俊
程春雷
杨昊
JIANG Jun;CHENG Chunlei;YANG Hao(Shandong Food and Drug Inspection and Research Institute(Key Laboratory for Research and Evaluation of Generic Drugs of National Medical Products Administration),Jinan,250000,China)
出处
《环境化学》
CAS
CSCD
北大核心
2024年第1期359-362,共4页
Environmental Chemistry
