QuEChERS-UPLC-MS/MS测定人参中19种植物生长调节剂残留及膳食暴露评估被引量：12

Determination of 19 Plant Growth Regulators in Ginseng and Dietary Exposure Assessment by QuEChERS-UPLC-MS/MS

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摘要利用QuEChERS-超高效液相色谱-串联质谱技术建立同时测定人参中19种植物生长调节剂残留的方法。样品经0.1%甲酸-乙腈涡旋提取,以0.01%甲酸水溶液-乙腈为流动相进行梯度洗脱,引入内标法进行辅助定量,选取Waters ACQUITY UPLC BEH C18色谱柱(50 mm×2.1 mm,1.7μm)进行分离,采用正负离子切换的质谱扫描模式进行监测。结果表明:19种化合物浓度在0.005 ng/mL~250 ng/mL时线性良好,相关系数R^(2)≥0.9911;精密度为1.09%~5.57%(n=6);定量限为0.05μg/kg~100μg/kg;采用3个浓度进行加样回收试验,回收率为74%~117%,相对标准偏差(relative standard deviation,RSD)不大于15%,符合方法学验证要求。对实际样品中检出的氯化胆碱、矮壮素、丁酰肼进行膳食暴露评估,3种化合物单一危害、总危害计算结果均小于1,膳食暴露风险处于可接受水平。 A method for the simultaneous determination of 19 plant growth regulators in ginseng by quick,easy,cheap,effective,rugged,and safe-ultra-high performance liquid chromatography tandem mass spectrometry(QuEChERS-UPLC-MS/MS)was established.Samples were extracted with acetonitrile containing 0.1%formic acid.Gradient elution was performed with 0.01%formic acid aqueous solution containing acetonitrile as the mobile phase.The analytes were separated on a Waters ACQUITY UPLC BEH C18 column and determined by the internal standard method.Nineteen compounds were simultaneously monitored by single injection using a MS acquisition method including both positive and negative experiments.The results were fairly linear ranging from 0.005 ng/mL to 250 ng/mL under the best conditions,with correlation coefficients≥0.9911.Precision was 1.09%to 5.57%(n=6).The limits of quantification were 0.05μg/kg to 100μg/kg.Recovery ranged from 74%to 117%with relative standard deviation≤15%at three concentration levels.The calculated hazard quotient and hazard index of choline chloride,chlormequat,and butanehydrazide detected in the actual samples were all<1,indicating that the dietary exposure risk was at an acceptable level.

作者彭韵洁陈丽娜杨明王奇时东方王晶刘春明 PENG Yun-jie;CHEN Li-na;YANG Ming;WANG Qi;SHI Dong-fang;WANG Jing;LIU Chun-ming(The Central Laboratory,Changchun Normal University,Changchun 130032,Jilin,China)

机构地区长春师范大学中心实验室

出处《食品研究与开发》 CAS 北大核心 2021年第24期161-169,共9页 Food Research and Development

基金吉林省教育厅“十三五”科学技术项目(JJKH20170658KJ) 吉林省科技发展计划项目(20200404020YY) 中央引导地方科技发展资金吉林省基础研究专项(202002049JC) 长春师范大学研究生科研创新项目([2020]第059号) 吉林省应用生态工程实验室自主创新能力建设(2108C0022) 长春师范大学自然科学基金项目(长师大自然合字[2016]第002号)。

关键词人参 QUECHERS 超高效液相色谱-串联质谱植物生长调节剂膳食暴露评估 ginseng QuEChERS ultra-high performance liquid chromatography tandem mass spectromentry plant growth regulator dietary exposure assessment

分类号 O657.63 [理学—分析化学] R284.1 [医药卫生—中药学]

作者简介彭韵洁(1995-),女(汉),硕士研究生,研究方向:分析化学;通信作者:刘春明(1964-),女,教授,博士,研究方向:天然药物分析。