高效液相色谱-电感耦合等离子体质谱法同时测定大气PM2.5中6种砷形态和2种铬形态的含量  

Simultaneous Determination of 6 Arsenic and 2 Chromium Species in Atmosphere PM2.5 by High Performance Liquid Chromatography- Inductively Coupled Plasma Mass Spectrometry

作　　者：花中霞[1] 马辉 王小青[1] HUA Zhongxia;MA Hui;WANG Xiaoqing(Shijiazhuang Technology Innovation Center for Chemical Poison Detection and Risk Early Warning,Shijiazhuang Center for Disease Control and Prevention,Shijiazhuang 0500ll,China)

机构地区：[1]石家庄市疾病预防控制中心,石家庄市化学毒物检测及风险预警技术创新中心,石家庄050011

出　　处：《理化检验（化学分册）》2022年第11期1249-1253,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：河北省医学科研重点课题(ZD20140147)。

摘　　要：提出了题示方法并用于大气PM2.5中砷胆碱(AsC)、砷甜菜碱(AsB)、三价砷[As(Ⅲ)]、二甲基砷(DMA)、一甲基砷(MMA)、五价砷[As(Ⅴ)]、三价铬[Cr(Ⅲ)]和六价铬[Cr(Ⅵ)]含量的同时测定。用采样器在固定监测点以石英滤膜在100 L·min^(-1)的流量下采集大气PM_(2.5)样品24 h,将滤膜等分为2份,其中一份剪碎后置于15 mL离心管中,加入6 mL含20 mmol·L^(-1)乙二胺四乙酸二钠的流动相B(在50 mmol·L^(-1)碳酸铵溶液中加入适量硝酸,使NO_(3)^(-)的物质的量达到碳酸铵溶液中NH_(4)^(+)物质的量的80%,用氨水将溶液酸度调节至pH 8.35),振荡30 min,过0.45μm滤膜,滤液进入高效液相色谱仪,其中各元素形态在HAMILTON PRP-X100色谱柱上用不同体积比的水和流动相B的混合溶液进行梯度洗脱分离,用电感耦合等离子体质谱仪测定^(75)As和^(52)Cr的含量。结果显示:在1.0~50.0μg·L^(-1)质量浓度范围内8种元素形态标准曲线的线性良好,方法检出限(3S/N)为0.003~0.025 ng·m^(-3);对空白样品进行加标回收试验,回收率为68.7%~112%,测定值的相对标准偏差(n=6)为1.4%~9.2%。方法用于石家庄市中部和东部区域采集的10个大气PM_(2.5)样品的分析,在10个样品中均检出了As(Ⅴ),检出量为0.74~2.35 ng·m^(-3);在东部区域采集的样品中还检出了少量AsB、As(Ⅲ)和Cr(Ⅲ);砷的检出量未超过GB 3095-2012规定的年均限值(6 ng·m^(-3))。The title method was proposed and used for simultaneous determination of AsC, AsB, As(Ⅲ), DMA, MMA, As(Ⅴ), Cr(Ⅲ) and Cr(Ⅵ) in atmosphere PM2.5. The atmosphere PM2.5samples were collected with quartz filter membrane by air sampler under condition of flow rate of 100 L·min-1for 24 h at a fixed monitoring point. The filter membrane was divided into two equal parts, one of which was cut into pieces and placed in a 15 mL-centrifugal tube. An aliquot(6 mL) of mobile phase B(an appropriate amount of nitric acid was added into 50 mmol·L-1ammonium carbonate solution, to make the molarity of NO3-reach 80% of that of NH4+, and the solution was adjusted to pH 8.35 by aqueous ammonia) containing 20 mmol·L-1ethylenediamine tetraacetic acid disodium salt was added, and the mixture was oscillated for 30 min. The extract was passed through a 0.45 μm filter membrane, and the filtrate was introduced into the high performance liquid chromatograph. The element species were separated on a HAMILTON PRP-X100 column by gradient elution of mixed solutions of water and mobile phase B at different volume ratios, and determined by inductively coupled plasma mass spectrometer in the form of75As and52Cr. The standard curves of the 8 element species showed the good linearity in the range of 1.0-50.0 μg·L-1, and detection limits(3 S/N) of the method were 0.003-0.025 ng·m-3. The recoveries obtained by the spiked recovery test were in the range of 68.7%-112%, with RSDs(n=6) of the determined values in the range of 1.4%-9.2%. Ten PM2.5samples collected from the central and eastern regions of Shijiazhuang city were analyzed by the prescribed method, and As(Ⅴ) was detected in each of the 10 samples with the detection amounts in the range of 0.74-2.35 ng·m-3. Small amounts of AsB, As(Ⅲ) and Cr(Ⅲ) were also detected in some samples collected from the eastern region, and detection amounts of arsenic did not exceed the annual limit(6 ng·m-3) specified by GB 3095-2012.

关 键 词：高效液相色谱-电感耦合等离子体质谱法 砷形态 铬形态 PM2.5 大气 

分 类 号：O657.73[理学—分析化学]