Determination of Au(III) and Pd(II) ions by flame atomic absorption spectrometry in some environmental samples after solid phase extraction

A simple and sensitive solid phase extraction method was developed for simultaneous separation and preconcentration of gold and palladium ions with N-(4-methylphenyl)-2-{[(4-phenyl-5-pyridine-4-yl-4H-1,2,4-triazol-3-yl)thio]acetyl}hydrazine carbo thioamide complex on Amberlite XAD-1180 resin before their determination by flame atomic absorption spectrometry. Some analytical parameters such as HNO₃ concentration of the sample solution, amount of complexing agent, sample volume, eluent type and volume, effects of foreign ions and adsorption capacity of the resin were investigated for quantitative recovery of gold and palladium ions. The effects of some anions and cations were also examined. Under optimum conditions, the detection limits for gold and palladium ions were found to be 0.29 and 0.19 μg L^?1, respectively. The preconcentration factor for gold and palladium was 250. After being validated by standard addition and analysis of standard reference material, the procedure was successfully applied to the analysis of sea and stream water, anodic slime, gold ore, soil and electronic waste.     

高效液相色谱串联质谱法测定环境水体中的全氟磺酸替代物

建立了高效液相色谱串联质谱同时分析环境水体中4种全氟磺酸污染物及4种替代物(3种全氟调聚磺酸及1种氯代多氟醚基磺酸)的分析方法.优化样品pH值、洗脱液用量等固相萃取(SPE)条件,并对萃取柱柱容进行了评估.采用亲水疏水平衡(HLB)固相萃取柱,在pH值为10的条件下对样品进行萃取,萃取柱干燥之后使用9 mL 甲醇作为洗脱液分3次对萃取柱进行洗脱.方法在0.150.0 ngmL-1范围内呈现良好的线性关系(r 0.998),方法检出限(S/N 3)为1.062 pgL-1,加标回收率53.2%134.1%.测定了来自4个不同地区的河水样品中全氟磺酸及替代物的残留水平.调聚磺酸类污染物中仅发现6:2 FTS的存在(0.20.6 ngL-1),而氯代多氟醚基磺酸在样品中都有检出(3.757.0 ngL-1).该方法简单、高效,可满足水体中全氟磺酸类污染物及其替代物的检测.     

超高效液相色谱-四极杆飞行时间质谱测定沉积物中4种氯酚类物质

建立了一种固相萃取（SPE）-超高效液相色谱（UPLC）-四极杆飞行时间质谱（Q-TOF）测定沉积物中4种氯酚类物质苄氯酚（CP）、二氯酚（DCP）、六氯酚（HCP）、溴氯芬（BCP）的分析方法.样品用1%甲酸丙酮超声提取,强阴离子交换固相萃取柱净化富集,以Waters HSS C18柱（2.1 mm×100 mm,1.8 μm）为分离色谱柱,采用0.004%甲酸水（V：V）-甲醇作为流动相进行梯度洗脱,采用四极杆飞行时间质谱检测.结果表明,六氯酚和溴氯芬在0.2-5 μg·L-1,二氯酚在0.4-20 μg·L-1,苄氯酚在2-100 μg·L-1的范围内线性关系良好,相关系数均大于0.99.在3个加标浓度水平下,回收率为69.5%-99.6%,相对标准偏差为3.4%-14.8%.方法准确灵敏,可满足沉积物中氯酚类物质的测定.     

QuEChERS-高效液相色谱-串联质谱法测定多果定在黄瓜和土壤中的残留及消解动态

建立了黄瓜和土壤样品中多果定的QuEChERS-高效液相色谱-电喷雾串联质谱（HPLC-ESI-MS/MS）检测方法,样品经甲醇（乙腈+甲醇）溶液,QuEChERS方法净化,以Agilent ZORBAX Eclipse Plus C18 （2.1 mm×50 mm,1.8 μm Rapid Resolution HD）色谱柱进行高效液相色谱分离,以电喷雾离子串联质谱正离子（ESI+）多反应监测（MRM）模式进行测定.多果定在黄瓜和土壤上的最低检出浓度（LOQ）为0.01 mg·kg-1,平均回收率为77.7%-113.4%,相对标准偏差（RSD）为1.5%-8.0%;多果定在黄瓜和土壤上的残留消解动态规律符合一级动力学方程,其半衰期分别为2.3-4.3 d和2.7-17.3 d.该方法样品前处理简单快速,分析时间短,灵敏度、准确度和精密度均符合农药残留检测要求,适用于黄瓜和土壤中多果定残留的检测.     

离子色谱与三重四极杆质谱TSQ Altis联用实现10种寡糖的同时分析检测

本文建立了针对10种寡糖,包括甘露糖醛酸（M）和古罗糖醛酸（G）的离子色谱串联三重四极杆质谱的分析方法。优化后的离子色谱条件：Thermo Scientific Dionex IonPac^TM AS19-4 μm (2 mm× 250 mm, Analytical),200 mmol·L⁻¹氢氧化钠-水为淋洗液,流速0.3 mL·min⁻¹,柱温30 ℃,电导检测器后连外接泵,三通阀加0.25 mL·min⁻¹乙腈。采用ESI源,扫描方式为选择反应检测。结果表明,离子色谱对不同聚合度的甘露糖醛酸和古罗糖醛酸有很好的保留和分离效果,三重四极杆质谱相比传统检测手段具有优异的灵敏度和高选择性;稳定性良好,连续进样5针,RSD均小于6.08%;标曲线性关系良好,R²≥0.9990;方法检出限0.34 μg·L⁻¹;加标回收率均≥90.2%,本方法可用于寡糖的定性及定量分析。     

超声提取辅助浸入式固相微萃取-气相色谱/质谱技术快速检测土壤中的有机氯农药残留

建立了超声提取辅助浸入式固相微萃取-气相色谱/质谱（DI-SPME-GC/MS）方法快速检测土壤中有机氯农残的新方法.该方法可实现分离、富集和进样一体化,减少样品前处理步骤.实验优化了DI-SPME的萃取条件、超声提取条件及GC/MS仪器参数.在优化条件下,9种OCPs在实验浓度范围（20—500 ng·g-1）内,线性关系良好,R2为0.9899—0.9987,方法检出限在0.67—1.76 ng·g-1,加标回收率在80.2%—117.1%,相对标准偏差（n=6）为10.0%—12.0%.结果表明该方法是一种简便快速、绿色环保的分析土壤中OCPs农残的方法.     

Assessment of potentially toxic elements in Swiss chard and sediments of Akaki River,Ethiopia

For the determination of 15 potentially toxic elements (V, Cr, Fe, Mn, Co, Ni, Cu, Zn, As, Se, Ag, Cd, Sn, Hg, and Pb) in plant and sediment samples of the Akaki River, Ethiopia, inductively coupled plasma–mass spectrometry, inductively coupled plasma–optical emission spectrometry, and a RA-915+ mercury analyzer were applied. Sediment and plant samples were mineralized using a closed-vessel microwave-assisted digestion system. The elemental concentrations varied considerably in plant and sediment samples. The minimum concentration was observed for known toxic elements (As, Hg, and Cd) while the highest concentration was observed for the elements of relatively low toxicity Zn, Mn, and Fe. The concentration of Cr, Fe, Pb, Zn, and As in Swiss chard surpassed the maximum permissible levels at specific sites. At some of the sites, the sediment quality guidelines are surpassed for Cu, Zn, and Pb.     

尘螨过敏原硝基化的位点选择性分析

过敏原的硝基化会引起其致敏潜能的增强,进而带来更大的致敏性健康风险. 过敏原蛋白质通常含有多个酪氨酸硝基化位点,分析过敏原硝基化的位点选择性是探究硝基化对过敏原致敏性影响的重要基础. 本文以尘螨过敏原为研究对象,建立了基于超高效液相色谱-串联质谱（UPLC-MS/MS）同时定量分析3种尘螨过敏原（Der f 1、Der p 1和Der p 2）的13个酪氨酸位点硝基化程度的方法,并应用于分析3种尘螨过敏原在过氧亚硝酸盐硝基化作用下的位点选择性. 结果表明,3种尘螨过敏原均发生了位点特异性的硝基化,Y₁₉₅、Y₃₇和Y₉₂分别为Der f 1、Der p 1和Der p 2中反应活性最高的硝基化位点. 尘螨过敏原位点选择性的硝基化表明,在评价硝基化尘螨过敏原的致敏性变化时应当考虑其位点特异性的硝基化状况.