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作 者:张春林[1] 高镯 王岩[1] 曹梦 马俊美[1] 张雷雷[1] 吴春敏[1] ZHANG Chunlin;GAO Zhuo;WANG Yan;CAO Meng;MA Junmei;ZHANG Leilei;WU Chunmin(Hebei Food Safety Key Laboratory,Hebei Food Inspection and Research Institute,Shijiazhuang 050200,China)
机构地区:[1]河北省食品安全重点实验室,河北省食品检验研究院,河北石家庄050200
出 处:《肉类研究》2021年第7期27-31,共5页Meat Research
基 金:国家市场监督管理总局技术保障专项(2019YJ009)。
摘 要:建立高效液相色谱-电感耦合等离子体-串联质谱法(high performance liquid chromatography-inductively coupled plasma tandem mass spectrometry,HPLC-ICP-MS/MS)测定水产品中5种形态砷的检测方法。利用MS/MS模式,以质量转移的方式消除干扰,流动相由10 mmol/L C_(2)H_(3)NaO_(2)、3 mmol/L KNO_3、12 mmol/L NaH_(2)PO_(4)等组成,采用梯度洗脱,As7阴离子交换色谱柱分离。结果表明:5种形态砷可完全分离,三价砷、二甲基砷、一甲基砷、五价砷和砷甜菜碱都具有良好的线性相关系数,检出限依次为0.00594、0.00528、0.00817、0.00841、0.01170 mg/kg,满足检测要求;加标回收率为83%~116%,相对标准偏差均小于5%;该方法具有简便快捷、准确度高、分离明显、检测效率高等特点,可对水产品中多种形态砷进行评价分析。In this study,an analytical method for the determination of five arsenic species in aquatic products by high performance liquid chromatography-inductively coupled plasma tandem mass spectrometry(HPLC-ICP-MS/MS)was established.In this method,interference was eliminated by means of mass transfer in the MS/MS mode.The mobile phase consisted of 10 mmol/L C_(2)H_(3)NaO_(2),3 mmol/L KNO_(3),and 12 mmol/L Na H_(2)PO_(4).Gradient elution was used for chromatographic separation on an As7 anion exchange column.Under these conditions,five arsenic species could be completely separated.The developed method exhibited good linearity for trivalent arsenic,dimethyl arsenic,monomethyl arsenic,pentavalent arsenic and arsenic betaine,and the detection limits were 0.00594,0.00528,0.00817,0.00841,0.01170 mg/kg,respectively,which met the analytical requirements.The spiked recoveries ranged between 83%and 116%,and the precision expressed as relative standard deviation(RSD)was less than 5%.This method had the characteristics of simplicity,rapidity,high accuracy,good separation,and high detection efficiency.It could be used to evaluate and analyze various species of arsenic in aquatic products.
关 键 词:高效液相色谱-电感耦合等离子体-串联质谱仪 水产品 形态砷 梯度洗脱 阴离子交换色谱柱
分 类 号:TS207.3[轻工技术与工程—食品科学]
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