清肺十八味丸中非法染色剂808猩红的测定  

Detection of illegally added 808 scarlet in Qingfei Shibawei Pills

作　　者：王秋实 王婷婷 李玲 陈乃江 WANG Qiushi;WANG Tingting;LI Ling;CHEN Naijiang(Food and Drug Control Center of Liangyungang City,Lianyungang 222000,China)

机构地区：[1]连云港市食品药品检验检测中心,连云港222000

出　　处：《西北药学杂志》2025年第2期10-15,共6页Northwest Pharmaceutical Journal

基　　金：国家药品监督管理局药品补充检验方法项目(编号:2022020)。

摘　　要：目的建立清肺十八味丸中非法染色剂808猩红的检测方法。方法高效液相色谱法(high performance liquid chromatography,HPLC)色谱柱为Phenomenex Gemini C_(18)柱(250 mm×4.6 mm,5μm);流动相为乙腈-体积分数0.1%甲酸(80∶20);检测波长为518 nm;柱温为30℃;进样体积为10μL;流速为1.0 mL·min^(−1)。高效液相色谱串联四极杆飞行时间质谱(high performance liquid chromatography with quadrupole time-of-flight mass spectrometry,HPLC-Q-TOF/MS)液相色谱柱为Poroshell 120 EC-C18(50 mm×3.0 mm,2.7μm);流动相为体积分数0.1%甲酸-乙腈(20∶80);进样体积为1μL;流速为0.2 mL·min^(−1);质谱离子源为正电子电喷雾电离(positive electrospray ionization,ESI^(+))。结果HPLC法测得808猩红在6.875~343.750 ng范围内线性关系良好(r=0.9996),平均加样回收率为98.76%,相对标准偏差(relative standard deviation,RSD)为1.22%(n=6)。LC/MS法测得供试品中相关离子峰及碎片特征与808猩红对照品一致。结论HPLC法操作简便,专属性强,重复性好,可用于清肺十八味丸中808猩红的初步确认,LC/MS法操作快速,可用于清肺十八味丸中808猩红的进一步确认,上述2种方法结合可用于清肺十八味丸的质量控制。Objective To establish a method for the detection of illegally added 808 scarlet in Qingfei Shibawei Pills.Methods High performance liquid chromatography(HPLC)method with a Phenomenex Gemini C_(18) column(250 mm×4.6 mm,5μm)was applied.The injection volume was 10μL at a flow rate of 1.0 mL·min^(−1) with acetonitrile-0.1%formic acid(80∶20)as mobile phase.The wavelength was set at 518 nm and the column temperature was 30℃.HPLC-quadrupole time-of-flight mass spectrometry(HPLC-Q-TOF/MS)method was performed on a Poroshell 120 EC-C18 column(50 mm×3.0 mm,2.7μm)in positive electrospray ionization(ESI^(+))mode,with acetonitrile-0.1%formic acid(80∶20)as mobile phase.The flow rate was 0.2 mL·min^(−1) and the column temperature was 30℃.Results In HPLC method,the linear range of 808 scarlet was between 6.875 and 343.750 ng(r=0.9996)with average recovery of 98.76%,RSD=1.22%(n=6).In LC/MS method,the molecular ion peaks and characteristic fragments in samples were consistent with those of the 808 scarlet control sample.Conclusion The HPLC method is easy to be operated,and it can achieve specificity and high repeatability,and can be used for the preliminary confirmation of Qingfei Shibawei Pills.The LC/MS method is fast and can be used for further confirmation of Qingfei Shibawei Pills.The combination of the above 2 methods can be used for the quality control of Qingfei Shibawei Pills.

关 键 词：清肺十八味丸 808猩红 含量测定 高效液相色谱法 四级杆飞行时间液质联用 

分 类 号：R927.2[医药卫生—药学]