摘要
建立了一种分析茶叶中高氯酸盐含量的固相萃取-高效液相色谱/串联质谱方法。样品采用50%甲醇溶液提取,C_(18)固相萃取柱净化,采用Phenomenex Luna Hillic色谱柱(100×2mm,3μm),流动相为5mmol/L乙酸铵水溶液(含0.2%甲酸)-甲醇,梯度洗脱,流速0.4mL/min。质谱采用多反应监测(MRM)模式检测,采用^(18)O标记高氯酸根离子作为内标进行基质校正,内标法定量。结果显示:高氯酸盐在1.0~20.0ng/mL范围内线性关系良好;对绿茶、乌龙茶、红茶3种茶叶样品的加标回收率为102.5%~105.3%,相对标准偏差(RSD)为1.2%~2.8%,定量限(S/N>10)为0.02mg/kg,检出限(S/N=3)为0.006mg/kg。实际样品检测表明该方法稳定、准确、可靠,适合于茶叶中高氯酸盐的测定。
An analytical method was developed using high performance liquid chromatography-tandem mass spectrometry for detecting the residues of perchlorate in tea.The perchlorate in tea was extracted with 50% methanol,purified with C18 solid-phase extraction（SPE）cartridge.The perchlorate was separated with a Phenomenex Luna Hillic column（100×2 mm,3μm）using（0.2% formic acid and 5 mmol/L ammonium acetate）-methanol as mobile phase at a rate of 0.4 mL/min.The perchlorate was analyzed by tandem mass spectrometry with negative ion electrospray under multiple reaction monitoring（MRM）mode.An ^（18）O-labelled perchlorate anion internal standard was used to correct matrix effects.Quantification analysis was conducted by the internal standard calibration.The results showed that the calibration curves of perchlorate were linear in the range of 1.0-20.0 ng/mL.The average recoveries of perchlorate in three kinds of tea（green tea,oolong tea and black tea）at three spiked levels were in the range of 102.5%-105.3%,with relative standard deviations of 1.2%-2.8%.The limits of quantitation and limits of detection were 0.02 mg/kg and 0.006 mg/kg,respectively.The proposed method was successfully applied in the detection of real sample with good stability.
作者
姚清华
柯秋璇
李捷
林虬
林永辉
颜孙安
YAO Qing-hua;KE Qiu-xuan;LI Jie;LIN Oiu;LIN Yong-hui;YAN Sun-an(Laboratory of Quality and Safety Risk Assessment for Agro-products,Ministry of Agriculture,Fuzhou 350003;Institute of Agricultural Quality Standards and Testing Technology Research,Fujian Academyof Agricultural Sciences,Fuzhou 350003;Technical Centre of Fujian Entry-Exit Inspection and Quarantine Bureau,Fuzhou 350001)
出处
《分析科学学报》
CAS
CSCD
北大核心
2018年第4期565-568,共4页
Journal of Analytical Science
基金
农业部茶叶质量安全风险评估项目(GJFP2017005)
福建省属公益类重点项目(2015R1025-2
2016R1024-1)
福建省农业科学院农产品质量安全创新团队项目(STIT2017-1-12)
福建省农业科学院青年英才基金项目(No.YC2017-8)
关键词
茶叶
高氯酸盐
固相萃取
高效液相色谱-串联质谱
残留分析
Tea
Perchlorate
Solid phase extraction
High performance liquid chromatography-tandemmass spectrometry
Residue analysis
作者简介
通讯作者：柯秋璇，女，硕士，工程师，从事食品理化分析研究．E-mail：connie4906@gmail．com
