HPLC-MS/MS法测定瓜蒌皮注射液中腺苷和唾液酸的含量  

Determination of the contents of adenosine and N-acetylneuraminic acid in Gualoupi injection by HPLC-MS/MS

作　　者：王辉俊 柯樱 叶冠 WANG Huijun;KE Ying;YE Guan(Shanghai Pharmaceuticals Holding Co.,Ltd.,Shanghai,201203,China)

机构地区：[1]上海医药集团股份有限公司,上海201203

出　　处：《上海医药》2018年第17期72-75,共4页Shanghai Medical & Pharmaceutical Journal

基　　金：上海市科委科研计划项目(15DZ1900100和15DZ1900101);中国博士后科学基金面上资助项目(2016M601637)

摘　　要：目的: 建立瓜蒌皮注射液中腺苷和唾液酸的HPLC-MS/MS定量分析方法。方法: 采用Waters Xbridge C18色谱柱(4.6 mm×50 mm,3.5 mm),流动相为甲醇-0.1%甲酸溶液,梯度洗脱。质谱条件为电喷雾离子源(ESI),负离子模式监测,源喷射电压:-4.500 k V;雾化温度:550℃,采用多反应监测模式(MRM)对瓜蒌皮注射液中腺苷和唾液酸进行定量分析。结果: 腺苷和唾液酸线性关系均良好(R≥0.995),线性范围均为250~32 000 nmol/L,腺苷和唾液酸的检出限分别为31.25 nmol/L和3.91 nmol/L。应用建立的HPLC-MS/MS方法测定了3批瓜蒌皮注射液中腺苷和唾液酸的含量,分别为1.407~1.465 mmol/L和251.0~678.7 nmol/L。结论: 该方法灵敏性、专属性和选择性好,可用于瓜蒌皮注射液中腺苷和唾液酸的定量测定和质量控制。Objective:To establish an HPLC-MS/MS method for the determination of adenosine and N-acetylneuraminic acid(NANA)in Gualoupi injection.Method:HPLC analysis was performed on a column of Waters Xbridge C18(4.6 mm×50 mm,3.5 mm)with linear gradient elution of methanol-0.1%formic acid solution.Mass spectrometry analysis was carried out at ion spray voltage of?4.500 kV and the turbo spray temperature of 550℃with electrospray ionization(ESI)ion source in negative mode.The contents of adenosine and NANA in Gualoupi injection were quantitatively determined by multiple reaction monitoring(MRM).Results:The standard curves of both adenosine and NANA showed good linearity(R≥0.995)over the range of 250-32 000 nmol/L and their detective limits were 31.25 nmol/L and 3.91 nmol/L.The contents of adenosine and NANA determined by HPLC-MS/MS in three batches of Gualoupi injections were 1.407-1.465 mmol/L and 251.0-678.7 nmol/L,respectively.Conclusion:This method possesses good sensitivity,specification and selectivity and can be used for the determination and quality control of adenosine and NANA in Gualoupi injection.

关 键 词：瓜蒌皮注射液 HPLC-MS/MS 腺苷 唾液酸 

分 类 号：TQ460.72[医药卫生—药物分析学] R286[化学工程—制药化工]