A method for the determination of methyl mercury (metHg),ethyl mercury (etHg),phenyl mercury (phHg) and inorganic mercury (Hg2+) in dried edible fungi by microwave extraction coupled with HPLC-ICP-MS was established.Microwave-acid extraction was selected as the sample pretreatment method by comparing the effects of different extraction methods.And the components of mobile phase used in the experiment were optimized,the separation of metHg,etHg,phHg and Hg2+ could be achieved within 12 min.Moreover,the linear regression equation was good(r>0.999 0),RSD≤10.0% and the limits of quantitation (LOQ) were 0.009,0.024,0.018 and 0.024 mg/kg,respectively.Furthermore,the recovery rates of boletus,Tricholoma matsutake and morchella esculenta were 77.5%-117.5%.The accuracy of the method was verified by two reference materials GBW10029 and Tort-3.Above all,the method is simple,effective,accurate,and suitable for the quantitative analysis of mercury in dried edible fungi.It provides a method basis for mercury speciation analysis in edible fungi and basic data for the determination of methylmercury limit value in edible fungi.
XIONG Shanbo
,
XIAO Quanwei
,
HE Jie
,
WANG Jialin
,
HE Hanting
,
LAN Hang
. Determination of mercury speciation in dried edible fungi by microwave extraction combined with HPLC-ICP-MS[J]. Food and Fermentation Industries, 2020
, 46(22)
: 252
-256
.
DOI: 10.13995/j.cnki.11-1802/ts.024746
[1] 王贤波,刘军波,余霞奎,等.微波萃取液相色谱－电感耦合等离子体质谱联用测定水产品中甲基汞、乙基汞和无机汞[J].安徽农业科学,2014(8):2 438-2 440.
[2] 刘娜,张兰英,杜连柱.高效液相色谱电感耦合等离子体质谱法测定汞3种形态[J].分析化学,2005,33(8):1 116-1 119.
[3] 刘丽萍,吕超,王颖.液相色谱-电感耦合等离子质谱联用技术测定水产品中汞化合物形态分析方法探讨[J].分析测试学报,2010,29(8):767-771.
[4] 张兰,陈玉红,王英峰,等.微波辅助萃取-高效液相色谱-电感耦合等离子体质谱法联用测定生物样品中的汞形态[J].环境化学,2013,32(11):2 219-2 222.
[5] 李妍,刘书娟,江冬青,等.气相色谱－电感耦合等离子体质谱联用技术应用于水产品中汞形态分析[J].分析化学,2008,6(6):793-798.
[6] 陈玉红,米健秋,张兰.高效液相色谱-电感耦合等离子体质谱联用测定环境水样中的二价汞、甲基汞、乙基汞与苯基汞[J].环境化学,2011,30(4):893-896.
[7] GB 5009.17—2014 食品安全国家标准 食品中总汞及有机汞的测定[S].北京:中国标准出版社,2014.
[8] 樊祥,张润何,刘博,等.高效液相色谱-原子荧光光谱法测定水产品中不同形态汞含[J].食品安全质量检测学报,2017,8(1):76-81.
[9] LEOPOLD K,FOULKES M,WBRSFOLD P J.Methods for the determination and speciation of mercury in natural waters-A review[J].Anal Chim Acta,2010,663(2):127-138.
[10] 梅光明,郭远明,张小军,等.浙江沿海海产品中汞形态分析测定与分布特征[J].食品科学,2015,36(24):229-234.
[11] 祖文川,汪雨,李冰宁,等.ICP-MS相关联用技术在食品元素形态分析中的应用及进展[J].质谱学报,2013,34(4):247-256.
[12] 毛永杨,杨桐,苏涛,等.高效液相色谱-原子荧光光谱联用法测定牛肝菌中无机汞、甲基汞、乙基汞的不确定度评估[J].食品科学,2017,38(24):272-276.
[13] KIM K H,KABIR E,JAHAN S A.A review on the distribution of Hg inthe environment and its human health impacts[J].Journal of Haz-Ardous Materials,2016,306:376-385.
[14] 刘庆阳,何滨,胡敬田,等.高效液相色谱与原子荧光光谱联用分析海产品中的甲基汞[J].分析试验室,2009,28(5):41-44.
[15] BROMBACH C C,GAJDOSECHOVA Z,CHEN BIN,et al.Direct online HPLC-CV-AFS method for traces of methylmercury without derivatisation:A matrix.independent method for urine,sediment and biological tissue samples[J].Anal Bioanal Chem,2015,407:973-981.
[16] BATISTA B L,ODRIGUES J L,SOUZA S S D,et al.Mercury speciation in seafood samples by LC-ICP-MS with a rapid ultrasound-assisted extraction procedure:Application to the determination of mercury in Brazilian seafood samples[J].Food Chemical,2011,126(4):2 000-2 004.
[17] 曹小丹,秦德元,郝伟,等.低压液相色谱-原子荧光快速测定鱼肉和土壤样品中的汞形态[J].分析化学,2017,42 (7):1 033-1 038.
[18] SHAQ A Q,KAZI T G,BAIG J A,et al.Simultaneously determination of methyl and inorganic mercury in fish species by cold vapor generation atomic absorption spectrometry[J].Food Chemistry,2012,134(4):2 345-2 349.
