高效液相色谱-电感耦合等离子体质谱法测定烟草及其制品中3种铅形态  

Determination of Three Lead Species in Tobacco and Tobacco Products by HPLC-ICP-MS

作　　者：吴若昕 田志章 张春涛[1] 田楠 邢立霞 李登科[1] 马立超[1] WU Ruoxin;TIAN Zhizhang;ZHANG Chuntao;TIAN Nan;XING Lixia;LI Dengke;MA Lichao(Tianjin Workstation,Technical Center,Shanghai Tobacco Group Co.,Ltd.,Tianjin 300163,China)

机构地区：[1]上海烟草集团有限责任公司技术中心天津工作站,天津300163

出　　处：《理化检验（化学分册）》2021年第7期621-626,共6页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：上海烟草集团有限责任公司科技项目(K2019-2-037P)。

摘　　要：建立了高效液相色谱-电感耦合等离子体质谱法(HPLC-ICP-MS)测定烟草及其制品中无机铅[Pb(Ⅱ)]、三甲基铅(TML)和三乙基铅(TEL)含量的方法。将烟草样品粉碎后,加入体积比为60∶40的1 mmol·L^(-1) 1-戊烷磺酸钠溶液和甲醇的混合溶液(流动相) 15 mL,于40℃超声萃取20 min,离心,上清液过0.22μm滤膜,用HPLC-ICP-MS测定滤液中3种铅形态含量。在烟草样品中加入硝酸和30%过氧化氢溶液,在程序升温条件下微波消解,消解液用水稀释后,用ICP-MS测定其中的铅总量。在HPLC分析中,在1.0 mL·min^(-1)流量下用流动相等度洗脱吸附在ZORBAX Eclipse Plus C18反相色谱柱上的3种铅形态,8 min即可实现高效分离。在ICP-MS分析中,同步监测206Pb、207Pb和208Pb等3种铅同位素,用三者含量和进行定量。结果显示:3种铅形态的质量浓度在0.5-50.0μg·L^(-1)内与其对应的质谱响应值呈线性关系,检出限(3S/N)为0.33-0.47μg·L^(-1);对实际样品进行3个浓度水平的加标回收试验,所得回收率为81.9%-96.5%,测定值的相对标准偏差(n=6)为5.3%-9.6%。方法用于烟叶样品和卷烟成品的分析,结果显示:烟叶样品及卷烟成品中均未检出有机铅,其铅形态以Pb(Ⅱ)为主,且含量较低(1.53-5.08μg·g^(-1));下、中、上部烟叶中铅含量呈递减分布;卷烟成品中的铅含量与烟叶样品的基本处于相同水平;检出的3种铅形态含量总和占铅总量的74.3%-84.6%。A method for the determination of inorganic lead[Pb(Ⅱ)],trimethyl lead(TML)and triethyl lead(TEL)in tobacco and tobacco products by HPLC-ICP-MS was established.After the tobacco sample was crushed,15 mL of the mixture(mobile phase)of 1 mmol·L^(-1) sodium 1-pentanesulfonate solution and methanol with volume ratio of 60∶40 was added.The sample was extracted by ultrasound at 40℃for 20 min and then centrifuged.The supernatant was filtered with a 0.22μm filtering membrane.The contents of the three lead species in the filtrate were determined by HPLC-ICP-MS.Tobacco samples were mixed with nitric acid and 30%hydrogen peroxide solution,and digested by microwave under the programmed temperature.The digestion solution was diluted with water and the total amount of lead was determined by ICP-MS.In HPLC analysis,the three lead species adsorbed on Eclipse plus C18 revesed-phase chromatographic column were isocratically eluted at a flow rate of 1.0 mL·min^(-1) within 8 min.In ICP-MS analysis,three lead isotopes,including 206Pb,207Pb and 208Pb,were simultaneously monitored and their total content was used for quantification.The results showed that the linearity relationships between mass concentrations of the three lead species and their respective MS response values were kept in the range of 0.5-50.0μg·L^(-1),with detection limits(3 S/N)in the range of 0.33-0.47μg·L^(-1).The spiked recovery test was made on actual samples at the 3 concentration levels,giving results of recovery in the range of 81.9%-96.5%,and RSDs(n=6)of the determined values ranged from 5.3%to 9.6%.The prescribed method was applied to the analysis of tobacco samples as well as cigarette samples,no organic lead was detected in the 2 kinds of samples.Pb(Ⅱ)was the main form of lead,with its content as low as 1.53-5.08μg·g^(-1).The content of lead in lower,middle and upper parts of tobacco samples decreased gradually.The lead content in cigarette samples was basically the same as that in tobacco samples.Sum of content of the three lead species ac

关 键 词：高效液相色谱-电感耦合等离子体质谱法 无机铅 三甲基铅 三乙基铅 形态分析 烟草 烟草制品 

分 类 号：O657.63[理学—分析化学]