基于特征性成分的肾石通颗粒中金钱草投料真实性考察  

Investigation of the Authenticity of Lysimachiae Herba Feeding in Shenshitong Granules Based on Characteristic Components

作　　者：胡亮 周明 王银红 罗疆南 孙辉 文庆 HU Liang;ZHOU Ming;WANG Yinhong;LUO Jiangnan;SUN Hui;WEN Qing(Hunan Institute for Drug Control,Changsha,Hunan,China 410001;Hunan Drug Inspection Center,Changsha,Hunan,China 410001;Hunan Drug Evaluation and Adverse Reaction Monitoring Center,Changsha,Hunan,China 410001)

机构地区：[1]湖南省药品检验检测研究院,湖南长沙410001 [2]湖南省药品审核查验中心,湖南长沙410001 [3]湖南省药品审评与不良反应监测中心,湖南长沙410001

出　　处：《中国药业》2023年第23期88-92,共5页China Pharmaceuticals

基　　金：湖南省自然科学基金[2022JJ80008]。

摘　　要：目的建立肾石通颗粒中广金钱草的掺伪检测方法。方法以常见混伪品广金钱草中夏佛塔苷为特征性成分,采用高效液相色谱-二极管阵列检测器(HPLC-PDA)法进行筛查与含量测定,色谱柱为Symmetry C_(18)柱(250 mm×4.6 mm,5μm),流动相为乙腈-0.1%磷酸溶液(10∶90,V/V),流速为1.0 mL/min,检测波长为340 nm,柱温为35℃。采用液相色谱串联质谱(HPLC-MS/MS)法进行确证试验,色谱柱为Ultimate LP-C_(18)柱(100 mm×2.1 mm,1.8μm),流动相为乙腈-10 mmol/L乙酸铵溶液(梯度洗脱),流速为0.2 mL/min,柱温为30℃;电喷雾负离子多反应监测模式,毛细管电压为3.5 kV,鞘气流速为11 L/min,辅助气流速为7 L/min,脱溶剂温度为300℃,离子传输管温度为350℃,以质荷比(m/z)563.0→353.0和563.0→383.0为特征离子对,碰撞能量为38 V和32 V。结果夏佛塔苷进样量在0.0308~0.6155μg范围内与峰面积积分值线性关系良好(R^(2)=0.9994,n=6);精密度、稳定性、重复性试验结果的RSD均低于2.0%(n=6);加样回收率为98.57%,RSD为1.03%(n=6)。222批次样品中,2批次样品检出并确证含有夏佛塔苷,含量分别为40.83,45.62μg/g。结论该方法重复性和稳定性好、结果准确,可作为肾石通颗粒中广金钱草掺伪投料的检测方法。Objective To establish a method for detecting the adulteration of Lysimachiae Herba in Shenshitong granules.Methods With schaftoside as the characteristic component in the common counterfeit product of Lysimachiae Herba,the high-performance liquid chromatography-photo diode array(HPLC-PDA)was used for screening and content determination.The chromatographic column was Symmetry C_(18)column(250 mm×4.6 mm,5μm),the mobile phase was acetonitrile-0.1%phosphoric acid solution(10∶90,V/V),the flow rate was 1.0 mL/min,the detection wavelength was 340 nm,and the column temperature was 35℃.The high-performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)method was used for confirmation,and the chromatographic column was Ultimate LP-C_(18)column(100 mm×2.1 mm,1.8μm),the mobile phase was acetonitrile-10 mmol/L ammonium acetate solution(gradient elution),the flow rate was 0.2 mL/min,and the column temperature was 30℃.Multi reaction monitoring(MRM)mode was adopted with electrospray negative ion(ESI-),the capillary voltage was 3.5 kV,the sheath gas flow rate was 11 L/min,the auxiliary gas flow rate was 7 L/min,the desolvent temperature was 300℃,the ion transfer tube temperature was 350℃,with mass charge ratio(m/z)563.0→353.0 and 563.0→383.0 as the characteristic ion pair,and the collision energies were 38 V and 32 V,respectively.Results The linear range of schaftoside was 0.0308-0.6155μg(R^(2)=0.9994,n=6).The RSDs of precision,stability,and repeatability test results were all lower than 2.0%(n=6).The recovery rate of schaftoside was 98.57%with an RSD of 1.03%(n=6).Among the 222 batches of samples,schaftoside was detected and identified in two batches,with contents of 40.83μg/g and 45.62μg/g,respectively.Conclusion This method is reproducible,reliable and accurate,which can be used as the detection method for the adulteration of Lysimachiae Herba in Shenshitong Granules.

关 键 词：肾石通颗粒 金钱草 广金钱草 夏佛塔苷 掺伪 安全监测 

分 类 号：R932[医药卫生—生药学] R286.0[医药卫生—药学]