超高效液相色谱串联质谱法测定腰息痛胶囊中龙胆苦苷含量  

Determination of Gentiopicroside in Yaoxitong Capsules by UPLC-MS/MS

作　　者：邓见春 邓杰华 周云峰 黄炳泉 王燕霞[3] DENG Jianchun;DENG Jiehua;ZHOU Yunfeng;HUANG Bingquan;WANG Yanxia(Gaoan People's Hospital,Yichun,Jiangxi,China 330800;The Inspection and Testing Center of Yichun,Yichun,Jiangxi,China 336000;The Fourth Affiliated Hospital of Nanchang University,Nanchang,Jiangxi,China 330003)

机构地区：[1]江西省高安市人民医院,江西宜春330800 [2]江西省宜春市检验检测中心,江西宜春336000 [3]南昌大学第四附属医院,江西南昌330003

出　　处：《中国药业》2024年第20期73-75,共3页China Pharmaceuticals

基　　金：江西省药品监督管理局科研项目[2021KY24]。

摘　　要：目的建立测定腰息痛胶囊中龙胆苦苷含量的超高效液相色谱串联质谱(UPLC-MS/MS)法。方法色谱条件,色谱柱为Waters ACQUITY UPLC®BEH C_(18)柱(100 mm×2.1 mm,1.7μm),流动相为0.1%甲酸溶液(含5 mmol/L乙酸铵)-乙腈(梯度洗脱),流速为0.3 mL/min,柱温为35℃,进样量为5μL;质谱条件,以m/z 401.0→179.0离子对为特征离子对,电喷雾离子源(ESI)、负离子扫描方式,多反应监测(MRM)模式。结果龙胆苦苷质量浓度在0.0551~22.0223μg/mL范围内与定量离子对峰面积线性关系良好,检测限为6.7 ng/mL;精密度、稳定性、重复性试验结果的RSD均小于2.1%。60批样品中龙胆苦苷的含量范围为27.66~3367.24μg/g,各生产企业间样品含量差异较显著。结论该方法操作简便,结果准确,精密度、重复性好,可用于腰息痛胶囊的质量控制。Objective To establish an ultra-high-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method for determining the content of gentiopicroside in Yaoxitong Capsules.Methods The UPLC chromatographic conditions were as follows:the chromatographic column was the Waters ACQUITY UPLC®BEH C_(18)column(100 mm×2.1 mm,1.7μm),the mobile phase was 0.1%formic acid solution(containing 5 mmol/L ammonium acetate)-acetonitrile(gradient elution),the flow rate was 0.3 mL/min,the column temperature was 35℃,and the injection volume was 5μL.The mass spectrometry conditions were as follows:the ion pair at the m/z 401.0→179.0 was the characteristic ion pair,the electrospray ion source(ESI)was adopted with negative ion scanning and multiple reaction monitoring(MRM)mode.Results The linear range of gentiopicroside was 0.0551-22.0223μg/mL,the limit of detection was 6.7 ng/mL.The RSDs of precision,stability and repeatability tests were all lower than 2.1%.The content of gentiopicroside in 60 batches of samples was in the range of 27.66-3367.24μg/g,and that was significantly different among various manufacturing enterprises.Conclusion This method is easy,accurate,precise and repeatable,which can be used for the quality control of Yaoxitong Capsules.

关 键 词：腰息痛胶囊 秦艽 龙胆苦苷 超高效液相色谱串联质谱法 含量测定 

分 类 号：R917[医药卫生—药物分析学] R927[医药卫生—药学]