Method Validation for the Determination of Tetrachlorodibenzodioxin at the Low Parts-per-Trillion Level

Gross, Michael L.; Sun, Tung; Lyon, P. A.; Wojinski, S F.; Hilker, David R.; Dupuy, Aubry E.; Heath, Robert G.

doi:10.1021/ac00235a600

Cited by 41 publications

(22 citation statements)

References 17 publications

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“…The classic example is the trace analysis of various chlorinated dioxins and dibenzofurans by GC/MS [1], a trace method that was validated over 20 years ago [2,3]. High resolving power also allows interferences to be excluded, especially when peak profiles are obtained [1,4].…”

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confidence: 99%

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Correction of accurate mass measurement for target compound verification by quadrupole time-of-flight mass spectrometry

Köfeler

Gross

2005

J. Am. Soc. Mass Spectrom.

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The aim of this work is to evaluate quadrupole/time-of-flight (QTOF) mass spectrometry for simultaneous measurement of accurate mass and quantification of a target by using a stable isotopically labeled internal standard. Mixtures of caffeine and 13 C 3 -caffeine (internal standard) at different concentration ratios were analyzed by capillary HPLC/QTOF. A calibration plot for quantification is linear over a factor of 20. Without invoking any correction scheme, the mass accuracy seriously degraded when the ratio of the mass standard to the test compound was not unity. The accuracy could be restored to approximately 2 ppm by using a quadratic function to correct the measured mass as a function of the measured signal ratio of target and internal calibrant. (J Am Soc Mass Spectrom 2005, 16, 406 -408)

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confidence: 99%

“…MS/MS is another means to achieve specificity, and the choice between it and accurate mass is one of the tradeoffs. Although a peak obtained at low resolving power can also give accurate mass, detection suffers because unresolved interferences can cause confusion [3,5].…”

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confidence: 99%

Correction of accurate mass measurement for target compound verification by quadrupole time-of-flight mass spectrometry

Köfeler

Gross

2005

J. Am. Soc. Mass Spectrom.

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“…After the interlaboratory validation, a detailed description of the successful GC/HRMS method and extraction approach was published (Gross et al, 1981). The method utilized bovine adipose tissue (10 g) spiked with 37 Cl‐TCDD (20 ng) as the internal standard and varying amounts of “native” TCDD for a calibration curve and for positive controls.…”

Section: Validation Of the Ms Methodsmentioning

confidence: 99%

The Development of a High‐resolution Mass Spectrometry Method for Ultra‐trace Analysis of Chlorinated Dioxins in Environmental and Biological Samples Including Viet Nam Era Veterans

Lay

Liyanage

Gidden

2020

Mass Spectrometry Reviews

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Chlorinated dioxins are labeled and recognized by both the World Health Organization and the United Nations Environmental Programme (UNEP) as “persistent organic pollutants”. Their potential for high toxicity is one of the primary factors behind intense public and regulatory scrutiny and the need to measure the compounds at very low limits, specifically the isomer 2,3,7,8‐tetrachlorodibenzo‐p‐dioxin (2,3,7,8‐TCDD). This article highlights the early mass spectrometry methods to investigate, detect, confirm, and quantify chlorinated dioxins and the initial applications involving human biomonitoring, as attempts were made to attribute health effects to TCDD exposure. This effort represented a complex and difficult scientific response to the pressing need to investigate expected exposures and alleged subsequent medical effects, which in the case of the Viet Nam veterans was being attempted a decade or more after their exposure. It is noteworthy that this method and its development touched on delicate issues involving human subjects, war veterans, environmental contamination, and was difficult not only scientifically, but for ethical and political reasons as well. Stable‐isotope dilution with analysis by gas chromatography/high‐resolution mass spectrometry (GC/HRMS) became the method of choice because of its ability to monitor characteristic ions and isotope ratios to quantify and qualify/confirm the analyte in the presence of coextracting and coeluting interferences at these low levels with the highest possible confidence. This method was rigorously tested and validated before it was used to discover and monitor levels in the environment and in various populations at then unprecedented low levels. These early studies demonstrated the feasibility of monitoring dioxins in humans even decades after exposure, and led to the detection of 2,3,7,8‐TCDD in the general population as well as specific overexposed populations. These studies also provided strong evidence regarding the origins of the 2,3,7,8‐isomer in the environment. © 2020 John Wiley & Sons Ltd. Mass Spec Rev

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“…Our specific goal was to assemble an instrument for analytical MS equipped with chemical ionization (CI), high resolving power, and accurate mass measurement and interface it with gas chromatography (GC) as a high-performance GC/ MS. At that time, I was working with the US EPA on validating the GC/MS analysis of 2,3,7,8-tetrachlordibenzodioxin, a highly toxic compound implicated in environmental exposure at Love Canal in NY, Times Beach in MO, and in the Vietnam war and alleged exposure in the lumber industry in Oregon (Gross et al, 1981;Heath et al, 1986). We understood the need of high resolving power and exact mass measurement in the GC mode for demanding environmental ultratrace analysis to maximize certainty in detection.…”

Section: A Ftms Team Nebraskamentioning

confidence: 99%

A Perspective on Personal Contributions to Ft‐icr Mass Spectrometry

Gross

Rempel

2020

Mass Spectrometry Reviews

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This is a personal perspective on our contributions to Fouriertransform ion cyclotron resonance (FT-ICR), including many early ones in a collaboration of Charles Wilkins and Michael Gross starting in the mid-1970s and then continuing for many years in a collaboration of Don Rempel and Michael Gross. The perspective is to honor Alan Marshall, who with Melvin Comisarow, first demonstrated FT-ICR mass spectrometry (MS) in 1974 (Comisarow & Marshall, 1974). Our intention is to review the contributions made together with Wilkins, Rempel, and a group of graduate and postdoctoral students, starting at the University of Nebraska-Lincoln and continuing here at Washington University in St. Louis. Besides offering a chance to reminisce about the early and exciting days of FT-ICR MS when academic laboratories were building and modifying mass spectrometers and other instruments, a nearly lost art, I am reminded of my editorship of this journal occurring over part of that time.

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Method Validation for the Determination of Tetrachlorodibenzodioxin at the Low Parts-per-Trillion Level

Cited by 41 publications

References 17 publications

Correction of accurate mass measurement for target compound verification by quadrupole time-of-flight mass spectrometry

Correction of accurate mass measurement for target compound verification by quadrupole time-of-flight mass spectrometry

The Development of a High‐resolution Mass Spectrometry Method for Ultra‐trace Analysis of Chlorinated Dioxins in Environmental and Biological Samples Including Viet Nam Era Veterans

A Perspective on Personal Contributions to Ft‐icr Mass Spectrometry

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