离子交换固相萃取-超高效液相色谱-串联质谱法测定减肥食品中p-辛弗林和去氧肾上腺素  

Determination of p-synephrine and phenylephrine hydrochloride in diet food by ion exchange solid-phase extraction coupled with ultra performance liquid chromatography-tandem mass spectrometry

作　　者：刘珈伶 LIU Jia-Ling(Guangxi-Asean Food Inspection Center,Nanning 530022,China)

机构地区：[1]广西-东盟食品检验检测中心,南宁530022

出　　处：《食品安全质量检测学报》2022年第20期6692-6698,共7页Journal of Food Safety and Quality

基　　金：2021年度广西壮族自治区市场监管局科技计划项目(GXSJKJ2021-1)。

摘　　要：目的 建立混合强阳离子交换固相萃取法(mixed mode cation exchange solid-phase extraction,MCX)-超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry UPLC-MS/MS)测定减肥食品中p-辛弗林和去氧肾上腺素两种辛弗林含量的分析方法 。方法 样品以50%甲醇为溶剂超声提取,离心后上清液经MCX固相萃取小柱净化,5%氨水甲醇洗脱,氮吹近干后初始流动相复溶以HSS T3色谱柱(100 mm×2.1 mm,1.8μm)分离,以0.1%(V:V)甲酸水溶液(含10 mmol/L乙酸铵)-乙腈作为流动相,进行梯度洗脱。在电喷雾正离子模式下,采用多反应监测(multiple reaction monitoring,MRM)模式,外标法定量。结果 p-辛弗林和去氧肾上腺素在1~100 ng/mL范围内与峰面积均成良好的线性,相关系数(r)均大于0.999。p-辛弗林和去氧肾上腺素的检出限均小于0.5μg/kg,定量限均小于1.0μg/kg,在咖啡、酵素粉、减肥茶和压片糖果4种减肥食品基质中1、2、10 ng/mL 3个水平下加标回收率为85.6%~110.4%,相对标准偏差均未超过5.0%(n=6)。结论 该方法 准确、可靠,可满足减肥食品中两种辛弗林的定量分析。Objective To establish an analytical method for the analysis of the concentration of p-synephrine and phenylephrine hydrochloride in diet foods by mixed mode cation exchange solid-phase extraction(MCX) coupled with ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). Methods The samples were extracted by ultrasound with 50% methanol as solvent. After centrifugation, the supernatant was purified by MCX solid-phase extraction column, and eluted with 5% ammonia and methanol. After nitrogen was nearly dried, the initial mobile phase was re-dissolved, separated by HSS T3 column(100 mm×2.1 mm, 1.8 μm), and subjected to gradient elution with 0.1%(V:V) formic acid aqueous solution(containing 10 mmol/L ammonium acetate)-acetonitrile as the mobile phase. Under the positive ion mode of electrospray ionization, multiple reaction monitoring(MRM) mode was adopted and quantification was conducted by external standard method. Results p-synephrine and phenylephrine hydrochloride exhibited good linearity over the range of 1-100 ng/mL with peak area, and the correlation coefficients(r) were greater than 0.999. The limits of detection of p-synephrine and phenylephrine hydrochloride were less than 0.5 μg/kg, and the limits of quantitation were less than 1.0 μg/kg. The recoveries of spiked samples at 1, 2 and 10 ng/mL in 4 kinds of weight loss food matrices including coffee, yeast powder, weight loss tea and tablet candy were 85.6%-110.4%, and the relative standard deviations were not more than 5.0%(n=6). Conclusion This method is accurate and reliable, and can be used for quantitative analysis of 2 kinds of synephrine in diet food.

关 键 词：p-辛弗林 去氧肾上腺素 减肥食品 混合强阳离子交换固相萃取法 超高效液相色谱-串联质谱法 

分 类 号：O657.63[理学—分析化学] TS218[理学—化学]