妇炎康复片中藏柴胡掺伪检查方法的建立  

Establishment of Identification Method for Adulterated Bupleurum marginatum in Fuyan Kangfu Tablets

作　　者：倪芹 来国防 NI Qin;LAI Guofang(Yunnan Institute for Food and Drug Control,Kunming,Yunnan,China 650106)

机构地区：[1]云南省食品药品监督检验研究院,云南昆明650106

出　　处：《中国药业》2025年第8期86-90,共5页China Pharmaceuticals

基　　金：云南省药品评价抽检专项[云药监办〔2023〕9号]。

摘　　要：目的建立妇炎康复片中藏柴胡掺伪的检测方法。方法采用超高效液相色谱-三重四极杆质谱联用法检测样品中尼泊尔柴胡皂苷K的含量,色谱柱为Waters CORTECS■C_(18)柱(150 mm×3.0 mm,2.7μm),流动相为0.1%甲酸溶液-0.1%甲酸乙腈溶液(70∶30,V/V),流速为0.25 mL/min,柱温为40℃,进样量为5μL;采用电喷雾(ESI)离子源,多反应监测模式(MRM)进行负离子扫描,以m/z 943.5→797.4为定量离子对。结果尼泊尔柴胡皂苷K质量浓度在0.010~10.026μg/mL范围内与峰面积线性关系良好(r=0.99919),检测限为0.040μg/g,定量限为0.12μg/g;精密度、稳定性、重复性试验结果的RSD均小于4.0%;平均加样回收率为84.61%,RSD为5.19%(n=9)。拟订样品中尼泊尔柴胡皂苷K的含量限度为35.0μg/g。29批次市售样品中,尼泊尔柴胡皂苷K含量为0.43~242.53μg/g;1批次超过含量限度,不合格率为3.45%。结论市售妇炎康复片整体质量较好,但个别批次存在藏柴胡掺伪现象。Objective To establish a detection method for identifying adulterated Bupleurum marginatum in Fuyan Kangfu Tablets.Methods The ultra-high-performance liquid chromatography-triple quadrupole mass spectrometry was used to determine the contents of nepasaikosaponin K in the samples.The chromatography column was the Waters CORTECS■C_(18) column(150 mm×3.0 mm,2.7μm),the mobile phase was 0.1%formic acid aqueous solution-0.1%formic acid in acetonitrile solution(70∶30,V/V),the flow rate was 0.25 mL/min,the column temperature was 40℃,and the injection volume was 5μL.The mass spectrometer was operated in negative ionization mode with multiple reaction monitoring(MRM),with m/z 943.5→797.4 as the quantitative ion pair.Results The linear ranges of nepasaikosaponin K was in the range of 0.010-10.026μg/mL(r=0.99919).The limit of detection was 0.040μg/mL and the limit of quantification was 0.12μg/mL.The RSDs of precision,stability and repeatability tests were all lower than 4.0%.The average recovery rates of the above four components was 84.61%,with RSD of 5.19(n=9).The specification for nepasaikosaponin K was established at 35.0μg/g as the acceptable threshold.The content of nepasaikosaponin K in 29 market samples were 0.43-242.53μg/g,non-compliance rate was 3.45%(1/29 batches exceeded the limit).Conlusion The overall quality of commercially available Fuyan Kangfu Tablets is satisfactory,but a few batches were found to contain adulterated Bupleurum marginatum.

关 键 词：妇炎康复片 藏柴胡 尼泊尔柴胡皂苷K 掺伪 超高效液相色谱-三重四极杆质谱法 

分 类 号：R917[医药卫生—药物分析学]