NQAD和ELSD在黄氏响声丸中贝母素甲和贝母素乙含量测定的对比研究  

doi:10.19778/j.chp.2024.06.001 A comparative study of NQAD and ELSD for the determination of peimine and peiminine in huangshi xiangsheng pills

作　　者：刘惠一 左利民[1] 仇小丹 郭鑫 连晓芳 贾庆莹 谷永升 刘宣麟 山广志[1] LIU Huiyi;ZUO Limin;QIU Xiaodan;GUO Xin;LIAN Xiaofang;JIA Qingying;GU Yongsheng;LIU Xuanlin;SHAN Guangzhi(Analysis and Testing Center of Institute of Medicinal Biotechnology,Chinese Academy of Medical Sciences and Peking Union Medical College,Beijing 100050,China;Xinjiang Medical University,Urumqi 830063,China;Key Laboratory for Traditional Chinese Medicine,Uyghur Medicine,Xinjiang Uygur Autonomous Region Institute of Pharmaceutical Research,Urumqi 830004,China)

机构地区：[1]中国医学科学院北京协和医学院医药生物技术研究所,北京100050 [2]新疆医科大学,乌鲁木齐830063 [3]新疆维吾尔自治区维吾尔药重点实验室,新疆维吾尔自治区药物研究所,乌鲁木齐830004

出　　处：《中国药品标准》2024年第6期529-535,共7页Drug Standards of China

基　　金：中国医学科学院中央级公益性科研院所基本科研业务费专项资金资助项目(2023-RW350-02);新疆维吾尔自治区重大科技专项项目(2022A03019-4)。

摘　　要：目的:采用纳克级水凝粒子激光计数检测器(nano quantity analyte detector,NQAD)测定黄氏响声丸中贝母素甲和贝母素乙的含量,并对NQAD和蒸发光散射检测器(evaporative light scattering detector,ELSD)的性能进行比较。方法:以CAPCELL PAK MGⅢC18色谱柱(4.6 mm×250 mm,5μm)为固定相,流动相为乙腈-水-二乙胺(65∶35∶0.03),流速为1.0 mL·min^(-1),柱温为25℃。结果:NQAD测得贝母素甲在2.450~1.470μg·mL^(-1)范围内其进样量与峰面积有良好的线性关系,相关系数为0.9993,检出限为14.70 ng,加样回收率为99.50%(n=9);贝母素乙在3.657~1.170μg·mL^(-1)范围内其进样量与峰面积有良好的线性关系,相关系数为0.9991,检出限为21.94 ng,加样回收率为100.5%(n=9)。ELSD检测贝母素甲和贝母素乙的检出限分别为24.50及36.57 ng;经双对数拟合线性范围分别为4.900~490.0、7.314~585.1μg·mL^(-1)。结论:与ELSD相比,NQAD测定贝母素甲及贝母素乙具有较高的准确度、精密度和灵敏度,动态线性范围更宽,可以直接通过线性回归进行含量计算,无需繁琐的双对数计算过程,数据处理更加高效,从而提升了分析方法的整体处理能力,能够更好满足黄氏响声丸中贝母素甲和贝母素乙的检测分析。Objective:The study aimed to quantify the contents of peimine and peiminine in huangshi xiangsheng pills using a nano quantity analyte detector(NQAD)and compare the results with the evaporative light scattering detector(ELSD).Methods:Analytical separation was conducted utilizing a CAPCELL PAK MGⅢC18 column(4.6 mm×250 mm,5μm)as the stationary phase.The mobile phase consisted of a mixture of acetonitrile-water-diethylamine(65∶35∶0.03),with a flow rate set at 1.0 mL·min^(-1) and the column maintained at a temperature of 25℃.Results:NQAD analysis revealed a robust linear correlation between the concentration and the peak area for peimine within a concentration range of 2.450 to 1.470μg·mL^(-1),achieving a correlation coefficient of 0.9993.The limit of detection(LOD)and recovery rate for peimine were determined to be 14.70 ng and 99.50%(n=9),respectively.Similarly,a linear relationship was observed for peiminine between the concentration and the peak area,spanning a range of 3.657 to 1.170μg·mL^(-1),with a correlation coefficient of 0.9991.The LOD and recovery rate for peiminine were 21.94 ng and 100.5%(n=9),respectively.In contrast,ELSD yielded LOD of 24.50 ng for peimine and 36.57 ng for peiminine,with linear range of double logarithmic fitting was 4.900 to 490.0μg·mL^(-1) and 7.314 to 585.1μg·mL^(-1),respectively.Conclusion:NQAD outperforms ELSD in the quantification of peimine and peiminine,offering superior accuracy,precision,and sensitivity,along with an extended dynamic linear range.By enabling direct content calculation via linear regression,it streamlines the process,bypassing the complex double logarithmic calculations.This approach not only boosts the efficiency of data handling but also substantially simplifies the computational steps,addressing the detection and analysis needs for peimine and peiminine in huangshi xiangsheng pills.

关 键 词：高效液相色谱 纳克级水凝粒子激光计数检测器 蒸发光散射检测器 黄氏响声丸 贝母素甲 贝母素乙 

分 类 号：R921.2[医药卫生—药学]