摘要
目的建立一种超高效亲水作用色谱串联三重四极杆质谱法(UHILIC-MS/MS),同时测定复方三维右旋泛酸钙糖浆中维生素B1、维生素B2、维生素B6、烟酰胺和泛酸钙的含量。方法采用超高效液相色谱仪,Waters ACQUITY BEHHILIC Amide色谱柱(2.1mm×100mm,1.7μm),以90%乙腈(含0.5%甲酸)-10mmol/L甲酸铵水(含0.5%甲酸)为流动相,进行梯度洗脱,流速0.30ml/min;在电喷雾(ESI)正离子模式下,用多反应监测(MRM)模式进行含量测定。结果在5min内,样品中5种维生素分别在各自考察的浓度范围内呈良好的线性关系,相关系数(r)均大于0.998 4;整体加样回收率在93.27%～100.39%之间,RSD为1.41%～4.96%;10批样品中维生素B1、维生素B2、维生素B6、烟酰胺、泛酸钙的含量测定结果分别为32.40～38.91、7.002～8.462、9.677～11.17、33.64～39.58、3.276～3.771mg/250g。结论本研究建立的UHILIC-MS/MS方法可快速实现对复方三维右旋泛酸钙糖浆中5种维生素类成分定性鉴定或定量检测,为复方三维右旋泛酸钙糖浆的开发利用和质量评价提供了可靠的技术检测方法。
Objective To establish a ultra hydrophilic interaction chromatography-tandem mass spectrometry（UHILICMS/MS）for the simultaneous determination of 5 B-vitamins including thiamine,riboflavin,pyridoxine,nicotinamide and calcium pantothenate in Compound Trivitamin and Calcium Pantothenate Syrup.Methods The chromatographic separation was performed on a Waters ACQUITY UHILIC BEH Amide（2.1 mm×100 mm,1.7μm）column with the mobile phase consisting of 10 mmol/L ammonium formate water and 90%acetonitrile both containing 0.5%formic acid water in a gradient elution at a flow rate of 0.30 ml/min.An electrospray positive ion multiple reaction monitoring（MRM）was used as a detector.ResultsFive B-vitamins in the sample achieved excellent linearity calibration curves over the concentration range tested（r〉0.998 4）within 5 min.The overall average recovery rates were in the range of 93.27%-100.39% with RSD of 1.41%-4.96%.The contents of thiamine,riboflavin,pyridoxine,nicotinamide and calcium pantothenate in ten samples were 32.40-38.91,7.002-8.462,9.677-11.17,33.64-39.58,3.276-3.771 mg/250 g,respectively.Conclusion The UHILIC-MS/MS method established in this study could quickly achieve qualitative identification or quantitative detection of five B-vitamins components in Compound Trivitamin and Calcium Pantothenate Syrup,which provided a reliable technical detection method for the development,utilization and quality evaluation of Compound Trivitamin and Calcium Pantothenate Syrup.
作者
任强强
赵优琴
许文
黄鸣清
叶水国
石贞香
REN Qiangqiang1,ZHAO Youqin1, XU Wen1 , HUANG Mingqing1 ,YE Shuiguo2, SHI Zhenxiang2(1 .School of Pharmacy , Fujian University of Traditional Chinese Medicine, Fujian Key Laboratory of Chinese Materia Medica, Fuzhou 350122, China; 2 .Sinopharm Xingsha Pharmaceuticals （Xiamen） Co. ,Ltd., Xiamen 361028, China)
出处
《药学实践杂志》
CAS
2018年第6期512-517,528,共7页
Journal of Pharmaceutical Practice
基金
国家自然科学基金面上项目(81673561)
福建省教育厅杰出青年人才项目
关键词
复方三维右旋泛酸钙糖浆
超亲水作用色谱-串联质谱
维生素B1
维生素B2
维生素B6
烟酰胺
泛酸钙
含量测定
Compound Trivitamin and Calcium Pantothenate Syrup
ultra hydrophilic interaction chromatography-mass spectrometry/mass spectrometry
thiamine
riboflavin
pyridoxine
nicotinamide
calcium pantothenate
content determination
