摘要
[目的]建立固相萃取液相色谱串联质谱法(LC-MS/MS)测定疏血通注射液中次黄嘌呤浓度。[方法]疏血通注射液经固相萃取柱处理后,采用LC-MS/MS进行含量测定。色谱柱为AcquityBEHC18分析柱(100mm×2.1mm,1.7μm),以甲醇-水(含0.1%甲酸)为流动相进行梯度洗脱,流速0.3mL/min。于ESI负离子模式下,以多反应离子监测(MRM)扫描方式进行监测,用于定量分析的离子为m/z134.9→92.0(次黄嘌呤)和m/z151.0→92.1(内标6-巯基嘌呤)。[结果]次黄嘌呤在质量浓度0.1~0.5μg/mL范围内与待测物和内标的峰面积比值呈良好线性关系(r=0.9998),平均加样回收率为98.7%,RSD为0.31%。[结论]该方法简便、准确、灵敏,可用于疏血通注射液中次黄嘌呤的浓度测定。
[Objective] Solid phase extraction with liquid chromatography-tandem mass spectrometry (SPE-LC-MS/MS) was applied to determine the concentration of hypoxanthine in Shuxuetong injection.[Methods] After extracted with SPE column,Shuxuetong injection was detected by LC-MS/MS. This injection was separated on an Acquity BEH C18 column (100 mm×2.1 mm,1.7 μm),and methanol-water (containing 0.1% formic acid) was used as a mobile phase for gradient elution at a flow rate of 0.3 mL/min. Mass spectrometric detection was performed in negative ion and multiple reaction monitoring mode with an electrospray ionization (ESI) source. The ion pairs used for quantitative analysis were m/z 134.9→92.0 for hypoxanthine and m/z 151.0→92.1 for 6-mercaptopurine (internal standard,IS).[Results] Hypoxanthine had a good linear relationship with the peak area ratio of the analyte and the IS in the range of 0.1~0.5 μg/mL (r=0.999 8). The average recovery rate was 98.7 %,and the RSD was 0.31%.[Conclusion] This method described here is a simple,accurate and sensitive method that can be used for the determination of hypoxanthine concentrationin Shuxuetong injection.
作者
王献瑞
赵西子
王晓明
郭亚卿
潘桂湘
黄宇虹
WANG Xianrui;ZHAO Xizi;WANG Xiaoming;GUO Yaqing;PAN Guixiang;HUANG Yuhong(Tianjin University of Traditional Chinese Medicine,Tianjin State Key Laboratory of Modern ChineseMedicine,Tianjin 300193,China;Second Affiliated Hospital of Tianjin University of TraditionalChinese Medicine,Tianjin 300250,China)
出处
《天津中医药大学学报》
CAS
2019年第5期478-481,共4页
Journal of Tianjin University of Traditional Chinese Medicine
关键词
液质联用
固相萃取
疏血通注射液
次黄嘌呤
定量分析
LC-MS/MS
solid phase extraction
Shuxuetong injection
hypoxanthine
quantitative determination
