三种固相萃取柱在农产品高氯酸盐检测中应用比较  

Comparison of Three Kinds of Solid Phase Extraction Columns in Perchlorate Determination in Agriculture Products

作　　者：李冬桂 吕丽兰[1,2,3] 陆覃昱 吴凤 李慧敏 黄婵婵[1,2,3] 陈羽烨 甘志勇 LI Donggui;LV Lilan;LU Qinyu;WU Feng;LI Huimin;HUANG Chanchan;CHEN Yuye;GAN Zhiyong(Guangxi Subtropical Crops Research Institute,Nanning,Guangxi 530001,China;Laboratory of Quality Risk Assessment for Agro-products(Nanning),Ministry of Agriculture and Rural Affairs,Nanning,Guangxi 530001,China;Quality Supervision and Testing Center of Subtropical Fruits and Vegetables,Ministry of Agriculture and Rural Affairs,Nanning,Guangxi 530001,China)

机构地区：[1]广西壮族自治区亚热带作物研究所,广西南宁530001 [2]农业农村部农产品质量安全风险评估实验室(南宁),广西南宁530001 [3]农业农村部亚热带果品蔬菜质量监督检验测试中心,广西南宁530001

出　　处：《农业研究与应用》2022年第6期44-52,共9页Agricultural Research and Application

基　　金：广西壮族自治区亚热带作物研究所科研业务费专项项目(桂热研201907);农产品质量标准及检测技术研究(桂农科2021YT148)。

摘　　要：为完善农产品中高氯酸盐的检测标准,本研究采用超高效液相色谱串联质谱仪进行测定,对比了HLB柱、C18柱和石墨碳黑柱对蔬菜、水果和茶叶中高氯酸盐检测的影响。结果表明,样品过净化柱后高氯酸盐及其内标峰形尖锐对称,HLB柱和C18柱均能获得较好的绝对回收率,绝对回收率分别为52.2%~101.0%和51.3%~99.9%,石墨碳黑柱绝对回收率最低,为29.4%~39.7%。对水果样品,HLB柱除色素效果优于C18柱,滤出液更澄清。因此,蔬菜、水果样品选HLB柱为净化柱。HLB柱和C18柱均能满足茶叶中高氯酸盐的测定,但C18柱价格更便宜,更适用于茶叶中高氯酸盐的检测。To improve standard of perchlorate determination in agricultural products,this paper used ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC―MS/MS) to compare effects of HLB column, C18 column and graphitized carbon black column on determination of perchlorate in vegetables, fruits and tea. The results showed that: after being filtered by the columns, narrow and symmetric peak of perchlorate and its internal standard appeared;high absolute recoveries were observed in HLB column and C18 column with their absolute recoveries of 52.2%―101.0% and 51.3%―99.9%, respectively, yet the minimum recovery was observed in graphitized carbon black column, 29.4%―39.7%. With HLB column better removed melanin in fruits than C18 column did as indicated by clearer filtrate. Therefore, for determining perchlorate in vegetable and fruit samples, HLB column was the better choice. Both HLB column and C18 column could be used for perchlorate determination in tea, but C18 column was cheaper than HLB column.

关 键 词：固相萃取 高氯酸盐 检测 高效液相色谱串联质谱 

分 类 号：O652.63[理学—分析化学]