Direct online quantitation of 2-methyl-3-methoxy-4-phenyl butanoic acid for total microcystin analysis by condensed phase membrane introduction tandem mass spectrometry

Duncan, Kyle D.; Beach, Daniel G.; Wright, Elliott J.; Barsby, Todd; Gill, Chris G.; Krogh, Erik

doi:10.1039/c8ay00516h

Cited by 7 publications

(8 citation statements)

References 37 publications

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“…There is a diverse range of other biochemical and biological assays capable of being used for analyses of MCs, which include protein phosphatase inhibition assay (Carmichael & An, 1999), conventional and quantitative real-time polymerase chain reaction (Lu et al, 2020), microarrays/DNA chips (Rantala, Rizzi, Castiglioni, De Bellis, & Sivonen, 2008), fluorimetric assays (Mak, Yeung, Kwok, Wong, & Wong, 2009), and other alternative biosensors (Feng, Zhu, Wang, & Shi, 2014;Shi et al, 2013;Yu, Jang, Kim, Kim, & Kim, 2011). Total MCs can also be measured by analyzing 3-methoxy-2-methyl-4-phenylbutyric acid (MMPB, an oxidation product of microcystins) using LC/MS/MS or other analytical techniques (Duncan et al, 2018;Foss & Aubel, 2015). However, these assays have had fewer applications than ELISA.…”

Section: Introductionmentioning

confidence: 99%

Microwave cell lysis for ADDA‐ELISA analysis of total microcystins and nodularins

Whitaker

Skibbe

et al. 2021

AWWA Water Science

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A fast and effective microwave treatment procedure was developed for the ADDA-enzyme-linked immunosorbent assay analysis of total extracellular and intracellular microcystins and nodularins in drinking water and ambient water. This microwave treatment procedure for a full batch of samples required 10-20 min versus the 3-4 hr typically needed for three freeze/thaw cycles. The obtained lowest-concentration minimum reporting level and method detection limit were 0.21 and 0.09 μg/L microcystin-LR (MC-LR) equivalents, respectively. Mean recoveries of 80%-92% with relative standard deviations of 4.2%-9.0% were obtained for all studied water matrices fortified at concentrations of 0.3-2.0 μg/L MC-LR. Compared with US Environmental Protection Agency Method 546, this alternate procedure provided more effective cell lysis and subsequently detected significantly higher concentrations of total microcystins and nodularins in a few water samples collected during harmful algal blooms, such as 61.0 versus 34.4 μg/L MC-LR equivalents in Lake Erie and 11.5 versus 9.1 μg/L MC-LR equivalents in an Indiana reservoir.

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Section: Introductionmentioning

confidence: 99%

Microwave cell lysis for ADDA‐ELISA analysis of total microcystins and nodularins

Whitaker

Skibbe

et al. 2021

AWWA Water Science

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“…In online condensed phase membrane introduction mass spectrometry (CP-MIMS) has been researched, which obviously avoids stability issues and importantly allows in situ analysis. 45,46 Matrices can suppress or enhance response during ionization, particularly in the ESI process, 7 therefore matrix effects were explored by comparing the response of spiked matrices samples with the standards response. The matrices included river, soil and WWTP samples.…”

Section: Methods Validationmentioning

confidence: 99%

An advanced LC–MS/MS protocol for simultaneous detection of pharmaceuticals and personal care products in the environment

Yao

et al. 2022

Rapid Comm Mass Spectrometry

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Rationale The development of appropriate analytical screening techniques for pharmaceuticals and personal care products (PPCPs) is the basis for studying the distribution and environmental impact of emerging contaminants (ECs). Mass spectrometry‐based screening methods vary with the complexity of the target compounds. It is challenging to balance both positive and negative ion quantification with a low detection limit. To establish a set of experimental methods including extraction, chromatography‐separation and mass spectrometry screening is one of the most important topics in PPCP research. This paper describes a universal and efficient qualification and quantification protocol for the simultaneous detection of 34 PPCPs in different environmental samples in a single analytical data acquisition run. Methods Thirty‐four representative PPCPs, which are widely distributed in the environment with high ecological toxicity and complex chemical structures, were selected as representative target ECs. The extraction of the target PPCPs was achieved using only one solid‐phase extraction cartridge without the need to adjust the pH of samples. The enriched samples were detected by LC–MS/MS in both positive and negative ion modes simultaneously. The protocol was evaluated based on the accuracy, precision, detection limits and matrix effects. Results This method achieved simultaneous detection of PPCPs in both positive and negative ion modes, with a single analytical cycle of 12 min. The observed SPE recoveries were between 40% and 115%. The instrumental detection limits (IDL) varied from 0.01 to 1 pg, and the method detection limits (MDL) were between 0.002 and 3.323 ng/l in different matrices. Most of the PPCPs were subjected to matrix suppression below 30%. The method was successfully applied for quantitative analysis of the PPCPs in different environmental samples, including river samples, wastewater treatment plant (WWTP) samples and soil samples. Conclusions This protocol developed a rapid and efficient detection method to simultaneous qualitative and quantitative 34 representative PPCPs in the environment. The IDL ranged from 0.01 to 1 pg and the MDL ranged from 0.002 to 3.323 ng/l in different matrices. The detection limit was one order of magnitude lower compared to previous studies. The protocol also provided a wide application range for different environmental matrices, which permitted the migration and transformation of PPCPs to be explored.

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“…However, several studies report better results using the negative ionization mode for MS/MS (207 → 131 transitions) [59,63,64,72,[85][86][87]. Some alternatives to the classical LC-MS/MS methods exist, namely laser diode thermal desorption-atmospheric pressure chemical ionization coupled to tandem mass spectrometry (LDTD-APCI-MS/MS) [66,79] and condensed phase membrane introduction mass spectrometry (CP/MIMS) [88]; both methods were applied to aqueous samples with a detection limit of 10 µg/L and 1 mg/L, respectively. Less commonly, other detection systems can be coupled to HPLC for the analysis of the MMPB product generated during Lemieux oxidation, HPLC with photodiode array detection (PDA) [89], HPLC with ultra-violet detection (UV) [63,67,69,90], or HPLC with fluorescence detection (FLD) [68].…”

Section: Analysis Of the Mmpb Productmentioning

confidence: 99%

“…Another strategy is to use an internal calibration via an internal standard (IS). For MMPB analysis, two IS can be used, 4-phenylbutyric acid (4-PB) [66,79,90] and isotopically-labeled MMPB (d3-MMPB) [84,88]. The first factor of choice between the two IS is the availability of the product; indeed, while 4-PB is easily available, d3-MMPB is more expensive and more difficult to obtain.…”

Section: Quantification Strategy (Internal Vs External Calibration)mentioning

confidence: 99%

Analysis of Total-Forms of Cyanotoxins Microcystins in Biological Matrices: A Methodological Review

Bouteiller

Lance

Guérin

et al. 2022

Toxins

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Microcystins (MCs) are cyclic heptapeptidic toxins produced by many cyanobacteria. Microcystins can be accumulated in various matrices in two forms: a free cellular fraction and a covalently protein-bound form. To detect and quantify the concentration of microcystins, a panel of techniques on various matrices (water, sediments, and animal tissues) is available. The analysis of MCs can concern the free or the total (free plus covalently bound) fractions. Free-form analyses of MCs are the most common and easiest to detect, whereas total-form analyses are much less frequent and more complex to achieve. The objective of this review is to summarize the different methods of extraction and analysis that have been developed for total forms. Four extraction methods were identified: MMPB (2-methyl-3-methoxy-4-phenylbutyric acid) method, deconjugation at basic pH, ozonolysis, and laser irradiation desorption. The study of the bibliography on the methods of extraction and analysis of the total forms of MCs showed that the reference method for the subject remains the MMPB method even if alternative methods and, in particular, deconjugation at basic pH, showed results encouraging the continuation of the methodological development on different matrices and on naturally-contaminated samples.

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Direct online quantitation of 2-methyl-3-methoxy-4-phenyl butanoic acid for total microcystin analysis by condensed phase membrane introduction tandem mass spectrometry

Abstract: Microcystins (MCs) are a potent class of hepatotoxins produced by several species of cyanobacteria, which have been responsible for illness and death in livestock and humans.

Cited by 7 publications

References 37 publications

Microwave cell lysis for ADDA‐ELISA analysis of total microcystins and nodularins

Microwave cell lysis for ADDA‐ELISA analysis of total microcystins and nodularins

An advanced LC–MS/MS protocol for simultaneous detection of pharmaceuticals and personal care products in the environment

Analysis of Total-Forms of Cyanotoxins Microcystins in Biological Matrices: A Methodological Review

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