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作 者:邓六爱 刘峰 张念英 郭冰 禚欢欢 DENG Liuai;LIU Feng;ZHANG Nianying;GUO Bing;ZHUO Huanhuan(Rizhao Inspection and Testing Center of Market Supervision Administration,Rizhao,Shandong 276800,China)
机构地区:[1]日照市市场监管检验检测中心,山东日照276800
出 处:《农产品加工》2021年第22期50-53,56,共5页Farm Products Processing
摘 要:建立了一种快速、准确测定茶叶中赤霉素含量的高效液相色谱-质谱定性定量检测方法。样品经0.1%的甲酸乙腈提取后,采用C_(18)柱吸附剂净化提取,C_(18)色谱柱分离,以5 mmol/L乙酸铵溶液(含0.1%甲酸)和乙腈为流动相进行梯度洗脱,电喷雾电离(ESI-),多反应监测模式扫描(MRM),基质外标法定量。结果表明,鲜叶和干茶中赤霉素在10.0~200.0 ng/mL质量浓度范围内呈线性相关,相关系数均大于0.999。鲜叶和干茶在3个水平的添加回收率分别为80.5%~98.5%,85.0%~106.0%,相对标准偏差(RSD)(n=6)均小于5%;定量限分别为3.31,0.88μg/kg。该方法操作简单、灵敏度和重复性好,能满足实际茶叶中赤霉素的检测。A rapid and accurate method using high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)was established for qualitative and quantitative determination of gibberellin in tea.The analyte was extracted from the samples by 0.1%formic acid acetonitrile,then purified by C18 adsorbent.The gibberellin was seperated by gradient elution with 5 mmol/L ammonium acetate and acetonitrile as the mobile phases.Mass spectrometry was conducted by electrospray ionization(ESI-)and multi response monitoring mode(MRM).The analyte was quantified by matrix external standard method.The results indicated that the calibration curve showed a good linearity of fresh leave and dry tea.The recoveries of fresh leaf and dry tea were 80.5%~98.5%and 85.0%~106%,respectively,and the relative standard deviation(RSD)(n=6)were less than 5%.The limits of quantification were 3.31 and 0.88μg/kg.This method was simple to operate with high sensitivity and good reproducibility.It could be used to test the gibberellin in tea.
关 键 词:茶叶 赤霉素 高效液相色谱-串联质谱(HPLC-MS/MS) 植物生长剂
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