摘要
建立一种能够同时测定保健食品中维生素B_(1)、维生素B_(6)、烟酸、烟酰胺和咖啡因含量的高效液相色谱-串联质谱法。以山楂酵母片、B族维生素片、多种B族维生素片、综合营养片(孕妇专用)、褪黑素片、多种维生素矿物质咀嚼片(儿童型)、黄山灵芝孢子粉、蜂胶软胶囊、保健口服液为试验材料,9种保健食品用去离子水溶解,滤液经色谱柱CAPCELL PAK C18(150 mm×2.1 mm,5μm)分离,流动相为0.1%甲酸溶液-0.1%甲酸甲醇溶液,梯度洗脱,采用电喷雾离子源正离子模式,检测方式为多重反应监测(MRM),喷雾电压为5000 V,离子源温度为500℃,对9种保健食品中的目标化合物进行分离测定。结果表明,维生素B_(1)、维生素B_(6)、烟酸、烟酰胺、咖啡因5种目标化合物在5~500μg/L的浓度范围内线性关系良好,R^(2)均大于0.9900,回收率在75.4%~94.5%,相对标准偏差(RSD)为1.1%~15.6%,维生素B_(1)、维生素B_(6)、烟酸、烟酰胺、咖啡因5种目标化合物的定量限分别为2.10、4.47、3.93、5.46、1.53μg/kg。该方法与现行国家标准相比,具有灵敏度高、前处理操作简单快速、抗干扰能力强,能同时测定不同剂型保健食品中5种目标化合物的含量。
A high-performance liquid chromatography tandem mass spectrometry method for the simultaneous determination of vitamin B_(1),vitamin B_(6),nicotinic acid,niacinamide,and caffeine in health foods was established.Hawthorn yeast tablets,B vitamins tablets,multi B vitamins tablets,comprehensive nutrition tablets(for pregnant women),melatonin tablets,multi vitamin mineral chewing tablets(for children),Mount Huangshan Ganoderma lucidum spore powder,propolis soft capsules,and health oral liquid were used as test materials.Nine kinds of health food were dissolved in deionized water,and the filtrate was passed through the chromatographic column CAPCELL PAK C18(150 mm×2.1 mm,5μm)to separate.Mobile phase was 0.1%formic acid solution-0.1%formic acid methanol solution.Gradient elution and positive ion mode of electric spray ion source were adopted.The detection mode was multiple reaction monitoring(MRM),spray voltage was 5000 V,the ion source temperature was 500℃,and the target compounds in 9 health foods were separated and determined.The results showed that the target compounds of vitamin B_(1),vitamin B_(6),Nicotinic acid,niacinamide,and caffeine had a good linear relationship at the concentration ranging from 5 to 500μg/L,with R^(2) all greater than 0.9900,recovery rates ranging from 75.4%to 94.5%,and relative standard deviation(RSD)ranging from 1.1%to 15.6%.The quantitative limits for the five target compounds of vitamin B_(1),vitamin B_(6),Nicotinic acid,niacinamide,and caffeine were 2.10,4.47,3.93,5.46,and 1.53μg/kg,respectively.Compared with existing national standards,this method had high sensitivity,simple and fast pre-treatment operation,and strong anti-interference ability,and could simultaneously determine the content of five target compounds in different dosage forms of health food.
作者
杨玉平
谢柏艳
YANG Yu-ping;XIE Bai-yan(Wuhan Institute for Drug and Medical Device Control,Wuhan 430075,China)
出处
《湖北农业科学》
2023年第9期124-129,共6页
Hubei Agricultural Sciences
基金
湖北省市场监督管理局2022年度科技计划项目(Hbscjg-KJ2022002)。
