高效液相色谱-电感耦合等离子体质谱联用法测定东海乌参样品中的二价汞、甲基汞、乙基汞和苯基汞.pdf

第7卷第11期
食品安全质量检测学报
Vol. 7 No. 11
2016年11月
ournal of Food Safcty and Qualily
Nov.2(016
高效液相色谱-电感耦合等离子体质谱联用法测定
东海乌参样品中的二价汞、甲基汞、
乙基汞和苯基汞
贾彦博1,陆吉琛,朱蓓,林舒忆,洪春来2
(1.杭州市食品药品检验研究院,杭州310022:2.浙江省农业科学院环境资源与土壤肥料硏究所杭州310021)
摘要:目的建立高效液相色谱-电感耦合等离子体质谱法( high performance liquid chromatography-inductively
coupled plasma- mass spcclromctry,IPLC-ICP-MS)测定东海乌参样品中的二价汞、甲基汞、乙基汞和苯基4
种汞形态的含量。方法样品经25%K()I微波萃取1h,采用 Agilent/ orhan Plus Cis色谱柱分离.,以10mmol
醋酸铵+0.12%-半胱氨酸缓冲盐及2%甲醇作为流动相进行梯度洗脱,采用ICP-MS进行检测。结果二价汞、
甲基汞、乙基汞和苯基汞在10min内完成分离,检出限分别为0.8、0.2、0.2和0.8ng/mL:在0.10、0.20和040
mgkg3个加标水平下,4种汞化合物的回收率为78.19%~105.8%,相对标准偏差为5.39%8.2%。结论本方法
简便、快速、准确,可适用于汞形态的分析。
关键词:高效液相色谱-电感耦合等离子体质谱法:二价汞;甲基汞;乙基汞;苯基汞;东海乌参
Determination of bivalent mercury, methyl-mercury, ethyi-mercury and
phenyi-mercury in Acaudina leucoproctu by high performance liquid
chromatography-inductively coupled plasma-mass spectrometr
JIA Yan-Bo、LUJi-Chen、 ZHU Bei、 LIN Shu-Yi、 HONG Chun-Lai
Hang hoa Instite or Hood and r g(ntrol, Hangzho 310022, China; 2. institute offmvironmen, Resorce
Soil and Fertilizer, Zheiiang Academy of agricultura Sciences, Hangshou 310021, China)
ABSTRACT: Objective To establish a method for determination of 4 kinds of mercury speciation including
bivalent mercury, methl-mercury, ethyl-mercury and phenyl-mercury in Acaudina leucoprocta by high performance
liquid chromatography-inductively coupled plasma-mass spectrometry (HIPLC-ICP-MS). Methods After
microwave extraction with 25% potassium hydroxide( KOH) for 1 h, the sample was separated by Agilent Zorbax
Plus C column with the mobile phase of 10 mmol. ammonium acctate/().12 /.-ystcincmethanol for gradicnt
elution and then detected by ICP-MS. Results Bivalent mercury, methi-mercury, ethyl-mercury and phenyl-mercury
could be separated within 10 min. The detect limits were 0.8, 0.2, 0.2 and 0.8 ng/ML, respectively. The recoveries of 4
kinds of mercury speciation spiked at 3 levels of 0.10, 0.20 and 0.40 mg/kg were ranged from 78.1% to 105.8% with the
relative standard deviations of 5.3"0-8.2%. Conclusion The developed method is simple, rapid and accurate, which
基金项目:浙江省公益性技术应用研究(分析測试)项目(2013C37058)
I und: Supported by the Project of hejian Province Public Welfare Technology Application Research(Analysis)(2013( 3705
通讯作者:洪春来,副研究员,主要研究方向为間体废弃物资源化利用与环境修复。IR-mail:82004897①q9com
Corresponding author: HONG hun-ai, Associate Professor Institut of Environment, Rcsourcc oil and Fcrtiizcr, Zhcjian Academy of
AgriculturalScicnccs,Hangzhou310021,ChinaE-mail:82998580(clqq.com
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