减肥类保健食品中非法添加物快速测定分析  

Rapid Determination and Analysis of Illegal Addition in Weight-loss Health Foods

作　　者：胡飞杰 王迪 余恒琳 朱毛毛 徐宁 王超璠 戴彩霞 Hu Feijie;Wang Di;Yu Henglin;Zhu Maomao;Xu Ning;Wang Chaofan;Dai Caixia(Nanjing Institute of Product Quality Inspection,Nanjing 210019,China)

机构地区：[1]南京市产品质量监督检验院,江苏南京210019

出　　处：《中国野生植物资源》2021年第11期32-39,共8页Chinese Wild Plant Resources

摘　　要：为了快速准确的检测出减肥类保健食品中的盐酸西布曲明、盐酸N-单去用基西布曲明、盐酸N,N-双去甲基西布曲明和酚酞,通过对色谱柱、流动相、柱温及流速等色谱条件的优化,建立了这4种非法添加物定性定量分析的最佳高效液相色谱方法,同时利用高效液相色谱-三重四级杆串联质谱联用仪对阳性样品进行进一步确证。结果表明:样品分析采用色谱柱为AgilentEclipsePlusC18(5μm,4.6×250 mm),流动相乙腈:0.02 mol/L乙酸铵水溶液(用乙酸调pH至4.0±0.2)为53∶47,柱温为50℃,流速为1.0 mL/min,盐酸西布曲明、盐酸N-单去甲基西布曲明、盐酸N,N-双去甲基西布曲明和酚酞4种物质在15 min内有良好的分离度,在5~100μg/mL范围内线性关系良好,4种物质的相关系数R^(2)≥0.999,检出限6.25~24.00 mg/kg,定量限20.80~80 mg/kg;验证试验表明,低、中、高3个水平的平均回收率分别为80.4%~104.6%,相对标准偏差为0.7%~9.5%。该方法准确度较高,可用于减肥类保健食品中盐酸西布曲明等4种非法添加物快速高效检测。In order to quickly and accurately detect sibutratmine byarochloride monohy-drate,didesmeth⁃yl sibutramine,N-didesmethyl sibutramine hyclrochloria and phenolphthalein,chromatographic column,chromatographic conditions,column temperature and flow rate were optimized to separate 4 illegal addi⁃tion.A qualitative and quantitive analysis method for simultaneous determination of 4 illegal addition by high performance liquid chromatography was established,and the positive samples were identified by ul⁃tra-high performance liquid chromatograph-tandem mass spectrometry.The analysis of samples was car⁃ried out on Agilent Eclipse Plus C18(5μm,4.6×250 mm)column with acetonitrile 0.02 mol/L ammonium acetatea queous solution(pH4.0±0.2)ratio 53∶47,column temperature was maintained at 50℃,at a flow rate of 1.0 mL/min.The results showed that sibutratmine hydrochloride monohydrate,didesmethyl sibutra⁃mine,N-didesmethyl sibutramine hydrochloride and phenolphthalein were well separated within 15 min,and had a good linear relationship in the range of 5-100μg/mL.The correlation coefficient(R^(2))was more than 0.999.The detection limit was between 6.25-24.00 mg/kg.The quantitative limit was between 6.25-24.00 mg/kg.The verification test shows that the average recovery of low,medium and high levels ranged from 80.4%to 104.6%.The relative standard deviation ranged from 0.7%to 9.5%.Thedeveloped method was accurate.It can be used for the determination of four drugs illegal addition in weight-loss health foods.

关 键 词：减肥保健食品 非法添加物 快速检测 高效液相色谱法 

分 类 号：TS207.3[轻工技术与工程—食品科学]