UPLC-MS/MS法同时测定金胆片中3种胆汁酸含量OA
Simultaneous Determination of Three Bile Aids in Jindan Tablets by UPLC-MS/MS Methods
目的:建立超高效液相色谱-串联质谱法快速检测金胆片中3种胆汁酸的含量.方法:金胆片经甲醇提取后,用ACQUITY UPLC®BEHC18色谱柱(100mm×2.1mm,1.7μm)进行色谱分离,流动相为甲醇-水(0.1%甲酸+5mmol/L乙酸铵),梯度洗脱.负离子模式下多反应监测模式检测.结果:牛磺猪去氧胆酸(THDCA)在0.103 3～51.650 0μg/mL、甘氨猪去氧胆酸(GHDCA)在0.102 5～51.250 0μg/mL、牛磺鹅去氧胆酸(TCDCA)在0.103 1～51.550 0μg/mL,线性关系良好(r≥0.999 5);方法重复性和准确度均良好(RSD≤3.75%);7家企业生产84批次金胆片中牛磺猪去氧胆酸、甘氨猪去氧胆酸、牛磺鹅去氧胆酸3种胆汁酸总量在2.088 0mg/g～6.921 6mg/g,按总量均值高低对企业排序为B>A>E>C>G>F>D.结论:该方法简单、快速、灵敏、准确,可用于金胆片中胆汁酸类成分的快速检测和质量评价.
Objective:To establish a rapid and accurate ultra-performance liquid chromatography-tandem mass spec-trometry(UPLC-MS/MS)method for the simultaneous determination of three bile acids in Jindan Tablets.Methods:Jindan Tablets was extracted with methanol.The chromatographic column was ACQUITY UPLC®BEHC18 column(100×2.1mm,1.7μm).Methanol-water(0.1%formic acid+5 mmol/L ammonium acetate was used as mobile phase for gradient elution.Detection was performed using an electrospray ionization source in negative ion mode with multiple reaction monitoring(MRM).Results:The peaks area of THDCA,GHDCA,and TCDCA had good linear rela-tionship with the quantity contents in the ranges of 0.103 3～51.650 0μg/mL,0.102 5～51.250 0μg/mL and 0.103 1～51.550 0μg/mL(r=0.9999,0.9995,0.9999),respectively.RSD of precision,reproducibility,stability tests and re-coveries rates were lower than 3.75%.The total content of THDCA,GHDCA,and TCDCA in 84 batches of Jindan Tablets from seven manufacturers ranged from 2.088 0 to 6.921 6 mg/g.Based on the mean total content,the manu-facturers were ranked as follows:B>A>E>C>G>F>D.Conclusion:The established method in this study is sim-ple,quick and accurate which is suitable for the rapid detection and quality evaluation of bile acids in Jindan Tablets.
王源潮;王天宇;旦增次旦;魏静;向虹蕾;贾巴将芬;罗霄;李文兵;达娃卓玛
西藏大学 医学院,西藏 拉萨 850000西南民族大学 青藏高原民族药用资源保护与利用国家民委重点实验室/四川省羌彝药用资源保护与利用技术工程实验室,四川 成都 610225西藏大学 医学院,西藏 拉萨 850000西南民族大学 青藏高原民族药用资源保护与利用国家民委重点实验室/四川省羌彝药用资源保护与利用技术工程实验室,四川 成都 610225西南民族大学 青藏高原民族药用资源保护与利用国家民委重点实验室/四川省羌彝药用资源保护与利用技术工程实验室,四川 成都 610225西南民族大学 青藏高原民族药用资源保护与利用国家民委重点实验室/四川省羌彝药用资源保护与利用技术工程实验室,四川 成都 610225成都市药品检验研究院 国家药品监督管理局中药材质量监测评价重点实验室,四川 成都 610045西南民族大学 青藏高原民族药用资源保护与利用国家民委重点实验室/四川省羌彝药用资源保护与利用技术工程实验室,四川 成都 610225西藏大学 医学院,西藏 拉萨 850000||西藏自治区食品药品检验研究院 国家药品监督管理局中药(藏药)质量控制重点实验室,西藏 拉萨 850000
医药卫生
超高效液相色谱-串联质谱法胆汁酸金胆片
UPLC-MS/MS MethodBile AcidJindan Tablets
《亚太传统医药》 2026 (3)
25-29,5
国家重点研发计划-中医药现代化专项(2023YFC3504101)四川省药品监督管理局项目(N5100012024000571)
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