摘要
目的建立高效液相色谱-串联质谱法同时定性和定量分析复合维生素片中叶酸和生物素的方法。方法样品用水溶液溶解,经Eclipse C18色谱柱(2.1 mm×100 mm,1.8μm)分离,流动相为0.1%甲酸溶液和乙腈梯度洗脱,流速0.2 ml/min,采用电喷雾离子源正离子模式,多反应监测(MRM)进行检测。结果叶酸和生物素在5 min内得到较好的分离。叶酸和生物素的线性范围分别为42~523和47~583 ng/ml,线性回归方程分别为y=1157.63x-6698.38(r^2=0.999 9)和y=207.93x-3052.26(r^2=0.998 2),低、中、高3个添加水平的回收率分别为99.9%~108.7%和90.1%~94.5%,相对标准偏差(RSD)均为1.0%(n=6),检出限分别为0.33和0.08μg/g。结论高效液相色谱-串联质谱法可靠、灵敏、准确,可用于复合维生素片中叶酸和生物素同时定性和定量分析。
Objective A method using high performance liquid chromatography tandem mass spectrometry for simultaneous determination of folic acid and biotin in compound vitamin pills was presented. Methods Samples were extracted by water. The analysis was carried out on an Agilent Eclipse C18（ 2. 1 mm × 100 mm,1. 8 μm） column with isocratic elution using a mobile phase of 0. 1% aqueous formic acid and acetonitrile at 0. 2 ml/min. Mass spectrometry acquisition was done in the positive ion mode and the analytes were detected in the multiple reaction monitoring（ MRM）mode. Results Folic acid and biotin in samples could be well separated within 5 min. The calibration cures were linear over the concentration range of 42-523 ng/ml and 47-583 ng/ml for folic acid and biotin,respectively. The linear regression equations were y = 1157. 63 x-6698. 38（ r^2= 0. 999 9） and y = 207. 93 x-3052. 26（ r^2= 0. 998 2）,respectively. The average recoveries were 99. 9%-108. 7% and 90. 1%-94. 5% for folic acid and biotin at low,medium and high adding levels,respectively. The relative standard deviation（ RSD） were both 1. 0%（ n = 6）. The detection limit was 0. 33 and 0. 08 μg/g for folic acid and biotin,respectively. Conclusion The developed method was precise,accurate and sensitive,which therefore could be applied for the analysis of folic acid and biotin in compound vitamin pills.
作者
王任
吴鸳鸯
程巧鸳
周明昊
WANG Ren;WU Yuan-yang;CHENG Qiao-yuan;ZHOU Ming-hao(Zhejiang Institute for Food and Drug Control, Zhejiang Hangzhou 310052, China)
出处
《中国食品卫生杂志》
北大核心
2018年第1期42-46,共5页
Chinese Journal of Food Hygiene
关键词
叶酸
生物素
高效液相色谱-串联质谱
复合维生素片
测定
Folic acid
biotin
high performance liquid chromatography-tandem mass spectrometry
compound vitamin pills
test
