Simultaneous determination of Hg(II) and alkylated Hg, Pb, and Sn species in human body fluids using SPME-GC/MS-MS

Dunemann, Lothar; Hajimiragha, Hossein; Begerow, Jutta

doi:10.1007/s002160051224

“…One of the most important parameters in the derivatization reaction is the pH. The effect of sample pH was investigated in urine and saliva samples and the optimum value was 5.3, which is in accordance with reported values [2,5,6,8]. At this pH the alkylation is achieved with maximum performance.…”

Section: Sample Preparationsupporting

confidence: 81%

“…Modern techniques applied for this purpose include gas or Liquid chromatography to separate various mercury species and subsequent detection by coupling one or more of several available detectors. Thus, GC hyphenation with MS [2 -5], MS/MS [6], ICP-MS [7 -10], GC-AFS [11 -13], or MIP-AED [9,14] are reported in the literature. Among them, GC-MS offers excellent sensitivity and selectivity with moderate cost and skill needs and is commonly used for mercury speciation.…”

Section: Introductionmentioning

confidence: 99%

Effect of sample matrix on sensitivity of mercury and methylmercury quantitation in human urine, saliva, and serum using GC‐MS

Zachariadis¹,

Kapsimali²

2008

J of Separation Science

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A rapid and sensitive method has been developed for the simultaneous determination of monomethylmercury (MMHg) and inorganic mercury (iHg) in human body fluids. The procedure is based on in situ derivatization of MMHg and iHg with sodium tetraethylborate (NaBEt(4)) directly in aqueous solutions followed by headspace solid phase microextraction (HS-SPME). The extracted species from spiked human urine, saliva, and serum are separated by capillary gas chromatography and detected by quadrupole MS (GC-MS). The optimization of the HS-SPME conditions like temperature, sample volume, extraction duration, and amount of alkylation agent, was performed in urinary solutions and aqueous solutions similarly buffered. The gas chromatographic conditions like injection temperature, helium flow rate, temperature program, and pressure conditions were also optimized. The recovery was ranged between 85 and 96% for MMHg and 88 and 98% for iHg. The LODs achieved were 10 and 15 ng/L for iHg and MMHg in urine, respectively, 54 and 60 ng/L for iHg and MMHg in saliva, respectively, and 61 and 81 ng/L for iHg and MMHg in serum, respectively. The RSD was ranged between 6.2 and 9.2% for MMHg and 5.0 and 8.2% for iHg.

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“…The preconcentration and speciation of Cr(III) and Cr(VI) in water sample can be performed using solid-phase extraction (SPE) [110]. An SPME (solid-phase microextraction) technique has been used as the sample preparation system for the innovative simultaneous multielement/multi-species determination of six different mercury, tin, and lead species in waters and urine with GC/MS-MS [146], [147]. The determination of arsenic species [As(III), As (V), MMA, DMA, arsenocholine, arsenobetaine)] has also been shown to work with an on-line digestion step prior to hydride generation AAS [130] (see Fig.…”

Section: Analysis Of Element Speciesmentioning

confidence: 99%

Sample Preparation for Trace Analysis

Begerow

¹

,

Dunemann

²

2006

Ullmann's Encyclopedia of Industrial Chemistry

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The article contains sections titled: 1. Introduction 1.1. A Strategy Appropriate to Trace Analysis 1.2. Avoidance of Systematic Errors 1.2.1. Trace Losses and Contamination 1.2.2. Uncertainty 2. Sample Preparation and Digestion in Inorganic Analysis 2.1. Sample Treatment after the Sampling Process 2.1.1. Stabilization, Drying, and Storage 2.1.2. Homogenization and Aliquoting 2.1.3. Requirements with Respect to Materials and Chemicals 2.2. Sample‐Preparation Techniques; General Considerations 2.2.1. Special Factors Associated with Microwave‐Assisted Digestion 2.2.2. Safety Considerations 2.3. Wet Digestion Techniques 2.3.1. Wet Digestion at Atmospheric Pressure 2.3.2. Pressure Digestion 2.3.2.1. Thermally Convective Pressure Digestion 2.3.2.2. Microwave‐Assisted Pressure Digestion 2.4. “Dry” Digestion Techniques 2.4.1. Combustion in Air 2.4.2. Combustion in Oxygen 2.4.3. Cold‐Plasma Ashing 2.4.4. Fusion 2.5. Illustrative Examples 2.5.1. Sample Preparation as a Function of Analytical Method 2.5.2. Combined Use of Multiple Decomposition Techniques 2.5.3. Comparative Merits of the Various Sample‐Preparation Techniques 2.5.4. Decomposition Procedures for Determining Nonmetals 2.6. Evaluation Criteria 2.6.1. Completeness 2.6.2. Uncertainty 2.6.3. Time Factors 2.6.4. The Final Result 2.7. Concentration and Separation of Inorganic Trace Materials 2.8. Automation and Direct Analysis 2.8.1. Automation 2.8.2. Direct Analysis 2.9. Analysis of Element Species 3. Sample Preparation in Organic Analysis 3.1. Sample Treatment after the Sampling Process 3.1.1. Stabilization, Drying, and Storage 3.1.2. Homogenization and Aliquoting 3.1.3. Requirements with Respect to Materials and Chemicals 3.2. Separation of the Analyte 3.2.1. Hydrolysis 3.2.2. Liquid ‐ Liquid Extraction 3.2.3. Soxhlet Extraction 3.2.4. Microwave‐Assisted Solvent Extraction 3.2.5. Supercritical Fluid Extraction (SFE) 3.2.6. Solid‐Phase Extraction (SPE) 3.2.7. Solid‐Phase Microextraction (SPME) 3.2.8. Stir‐Bar Adsorptive Extraction (SBSE) 3.2.9. Miscellaneous Techniques 3.3. Headspace Techniques 3.3.1. Static Headspace Technique 3.3.2. Dynamic Headspace Technique (Purge and Trap) 3.4. Determination of Trace Organic Materials in Air Samples 3.5. Analyte Concentration 3.6. Derivatization 3.7. Coupled Techniques Trace analysis is a very relevant and applications‐oriented branch of analytical chemistry. The sample preparation for trace analysis must be custom‐tailored to the problem at hand. Systematic errors can arise by contact with vessel materials, reagents, or the ambient atmosphere, as well as any change in chemical or physical state. In inorganic analysis, sample preparation has to meet the requirements for a substantially trouble‐free determination of the analyte. Digestion of the matrix (microwave digestion, wet digestion, dry digestion techniques) and subsequent careful comparison of several decomposition techniques is therefore an essentially important step. Some separation and concentration techniques of the analytes are liquid –liquid extraction, solid‐phase extraction, special precipitation reactions, and electrolytic deposition. The introduction of laboratory robots should make it possible to incorporate a significant degree of automation into the time‐consuming, labor‐intensive area of sample preparation as well, leading to more efficient, reliable, and reproducible sample work‐up. The goal of sample preparation in organic trace analysis is to isolate the analyte from the sample matrix (e.g., liquid‐liquid extraction, Soxhlet extraction, microwave‐assisted solvent extraction, steam distillation) and then concentrate it and convert it into a form suitable for analysis by the selected method. Separation and concentration of an analyte must often be followed by some type of derivatization. Various coupled sample preparation and determination processes are increasingly utilized in trace organic analysis.

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“…58 So far, few have used SPME to analyse endogenous compounds in biological matrices. Reported applications include quanti¢cation of trimethylamine in urine for diagnosis of inherited trimethylaminuria (¢sh odour syndrome), 52 analysis of urinary organic acids, 59 steroids 60 and volatile compounds in a variety of metabolic disturbances, 61 volatile compounds in blood, 62 isoprene 63 and formaldehyde in breath 64 and volatile fatty acids in faeces.…”

Section: 7mentioning

confidence: 99%

“…Covalent a¤nity chromatography with thiol^disul-phide interchange SPE was used to extract metallothionein and metals from physiological £uids, 81 and headspace SPME was used in a GC/MS^MS method to measure Hg 2+ and alkylated Hg, Pb and Sn as tetraethylborate complexes. 58 There may be a place for SPE and SPME in clinical trace-metal analyses, particularly in speciation studies.…”

Section: The Futurementioning

confidence: 99%

Solid-phase extraction in clinical biochemistry

Walker

¹

,

Mills

²

2002

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In order to measure low concentrations of analytes in plasma and urine, it is often necessary to extract and concentrate them. With solid-phase extraction (SPE), this is achieved by partitioning the analytes between a solid and a liquid or headspace vapour. A wide range of high-quality materials is now available to do this, offering a variety of separation modes for different applications. These include partitioning using reversed-phase, normal-phase, ion-exchange, restricted-access and immunoaf nity sorbents or molecularly imprinted polymers and, increasingly, combinations of these processes. Solid-phase microextraction was introduced to analyse volatile and semivolatile compounds. The range of sampling formats has expanded from simple packed syringes to cartridges, disks, SPE pipette tips and 96-well plates. These developments have facilitated automated off-and on-line sample processing. The basic principles of SPE and the recent innovations are reviewed here. This is a technological growth area. Some of the developments are nding application in clinical toxicology. However, they could also be of wider value in clinical chemistryfor example, for analyses of volatile and non-volatile metabolites, peptides, radioactive elements and trace metal speciation.

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Simultaneous determination of Hg(II) and alkylated Hg, Pb, and Sn species in human body fluids using SPME-GC/MS-MS

Cited by 74 publications

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Effect of sample matrix on sensitivity of mercury and methylmercury quantitation in human urine, saliva, and serum using GC‐MS

Effect of sample matrix on sensitivity of mercury and methylmercury quantitation in human urine, saliva, and serum using GC‐MS

Sample Preparation for Trace Analysis

Solid-phase extraction in clinical biochemistry

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