Microchimica Acta, volume 188, issue 5, publication number 152

LC-MS analysis of nitroguanidine compounds by catalytic reduction using palladium modified graphitic carbon nitride catalyst

Nikolaev V S ¹

Sladkevich Sergey ¹

Divina Uliana ¹

Prikhodchenko Petr V. ²

Gasser Guy ^{1, 3}

Falciola Luigi ⁴

Longhi Mariangela ⁴

Lev Ovadia ¹

Hide authors affiliations Show authors affiliations: 4 affiliations

The Institute Chemistry, The Casali Center of Applied Chemistry, The Hebrew University of Jerusalem, Jerusalem, Israel |

Kurnakov institute of General and Inorganic Chemistry, Russian Academy of Sciences, Moscow, Russia |

Water Monitoring Laboratory, Israel Water Authority, Rishon Lezion, Israel |

⁴

Dipartimento Di Chimica, Università Degli Studi Di Milano, Milan, Italy |

Publication type: Journal Article

Publication date: 2021-04-04

Springer Nature

Journal: Microchimica Acta

Quartile SCImago

Quartile WOS

Impact factor: 5.7

ISSN: 00263672, 14365073

DOI: 10.1007/s00604-021-04814-0

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Analytical Chemistry

Abstract

The analysis of compounds of the nitroguanidine family at trace level poses an analytical challenge. Nitroguanidine, 1-methyl-3-nitroguanidine, and 1-methyl-3-nitro-1-nitrosoguanidine, which are addressed in this article, have low lipophilicity, with log(Kow) equal to −0.89, − 0.84, and 0.68, respectively, and as such are not amenable for preconcentration from water. Liquid-liquid extraction and SPE fail to concentrate them from water and it is also not possible to extract them by ion exchange resin even after a pH change. Nitroguanidine and 1-methyl-3-nitroguanidine nitramines are explosives of growing use and thereby growing environmental concern due to lower detonation sensitivity compared to RDX. A sensitive method for the determination of nitroguanidine, 1-methyl-3-nitroguanidine, and 1-methyl-3-nitroso-1-nitroguanidine by reduction to the respective amines and subsequent hydrophobization by derivatization with 4-nitrobenzaldehyde followed by LC-ESI-MS analysis is described. Reduction by sodium borohydride using palladium modified graphitic carbon nitride (Pd/g-C3N4) provided improved sensitivity compared to the traditional palladium modified activated carbon due to the lower adsorption of the reduction products on the carbon nitride substrate. The limit of detection of the method was 10 ng L−1 for nitroguanidine, and repeated analyses of spiked effluents and contaminated spring water gave relative standard deviations of 8.8% and 6.5%, respectively. The findings illuminate the great promise of Pd/g-C3N4 as a reduction catalyst for the determination of challenging hydrophilic organic contaminants.

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Nikolaev V. S. et al. LC-MS analysis of nitroguanidine compounds by catalytic reduction using palladium modified graphitic carbon nitride catalyst // Microchimica Acta. 2021. Vol. 188. No. 5. 152

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Nikolaev V. S., Sladkevich S., Divina U., Prikhodchenko P. V., Gasser G., Falciola L., Longhi M., Lev O. LC-MS analysis of nitroguanidine compounds by catalytic reduction using palladium modified graphitic carbon nitride catalyst // Microchimica Acta. 2021. Vol. 188. No. 5. 152

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TY - JOUR

DO - 10.1007/s00604-021-04814-0

UR - https://doi.org/10.1007%2Fs00604-021-04814-0

TI - LC-MS analysis of nitroguanidine compounds by catalytic reduction using palladium modified graphitic carbon nitride catalyst

T2 - Microchimica Acta

AU - Nikolaev, V S

AU - Sladkevich, Sergey

AU - Divina, Uliana

AU - Prikhodchenko, Petr V.

AU - Falciola, Luigi

AU - Longhi, Mariangela

AU - Lev, Ovadia

AU - Gasser, Guy

PY - 2021

DA - 2021/04/04 00:00:00

PB - Springer Nature

IS - 5

VL - 188

SN - 0026-3672

SN - 1436-5073

ER -

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@article{2021_Nikolaev,

author = {V S Nikolaev and Sergey Sladkevich and Uliana Divina and Petr V. Prikhodchenko and Luigi Falciola and Mariangela Longhi and Ovadia Lev and Guy Gasser},

title = {LC-MS analysis of nitroguanidine compounds by catalytic reduction using palladium modified graphitic carbon nitride catalyst},

journal = {Microchimica Acta},

year = {2021},

volume = {188},

publisher = {Springer Nature},

month = {apr},

url = {https://doi.org/10.1007%2Fs00604-021-04814-0},

number = {5},

doi = {10.1007/s00604-021-04814-0}

}

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Publisher

Springer Nature

Journal

Microchimica Acta

Quartile SCImago

Quartile WOS

Impact factor

5.7

ISSN

00263672 (Print)
14365073 (Electronic)

Labs

Laboratory of peroxide compounds and materials based on them

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