Determination of Three Benzalkonium Chloride Homologues in Environmental Water by Ultra High Performance Liquid Chromatography- Quadrupole/Electrostatic Field Orbitrap High Resolution Mass Spectrometry

DONG Huijun; MA Tianyi; LI Yi; BAI Xueshan; DONG Jianfang; ZHANG Lu

doi:10.15898/j.cnki.11-2131/td.202201190015

Rock and Mineral Analysis > 2022 > 41(6): 1050-1059. > DOI: 10.15898/j.cnki.11-2131/td.202201190015

DONG Huijun, MA Tianyi, LI Yi, BAI Xueshan, DONG Jianfang, ZHANG Lu. Determination of Three Benzalkonium Chloride Homologues in Environmental Water by Ultra High Performance Liquid Chromatography- Quadrupole/Electrostatic Field Orbitrap High Resolution Mass Spectrometry[J]. Rock and Mineral Analysis, 2022, 41(6): 1050-1059. DOI: 10.15898/j.cnki.11-2131/td.202201190015

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Determination of Three Benzalkonium Chloride Homologues in Environmental Water by Ultra High Performance Liquid Chromatography- Quadrupole/Electrostatic Field Orbitrap High Resolution Mass Spectrometry

Hebei Geological Environment Monitoring, Hebei Key Laboratory of Geological Resources and Environment Monitoring & Protection, Shijiazhuang 050021, China

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Received Date: January 18, 2022
Revised Date: May 09, 2022
Accepted Date: July 14, 2022
Available Online: December 13, 2022

Abstract

ABSTRACT

BACKGROUND
Benzalkonium chloride has a non-oxidizing bactericidal effect and is widely used in medical and health service. With the discharge of sewage into the environment, benzalkonium chloride has been identified as a harmful compound that may seriously inspect susceptible organisms in the ecosystem. Exact quantitative analysis of benzalkonium chloride in environmental water is of great significance for human and ecological environmental health. However, low content of benzalkonium chloride exist in environmental water. The interference of a complex matrix causes false positive results to occur easily. Therefore, the detection method is required to have lower detection limits and more accurate qualitative analysis ability.
OBJECTIVES
To establish a method for the determination of three benzalkonium chloride homologues (n-C₁₂H₂₅-C₉H₁₃NCl, n-C₁₄H₂₉-C₉H₁₃NCl, n-C₁₆H₃₃-C₉H₁₃NCl) in environmental water.
METHODS
Ultra-high performance liquid chromatography quadrupole/electrostatic field orbitrap high resolution mass spectrometry (UPLC-Q-Orbitrap HRMS) was used. The sample was filtered through a 0.22μm membrane, and then mixed with the same volume of methanol. The mobile phase consisted of 10mmol/L ammonium acetate aqueous solution which contained 1% (V/V) triethylamine as mobile phase B and methanol as phase A, with gradient elution. Accucore C18 column (150mm×2.1mm, 2.6μm) was used to separate the baseline of three benzalkonium chloride within 6 minutes, and the data were collected by electrostatic field orbitrap mass spectrometry in SIM mode at 60, 000 resolution.
RESULTS
The contents of three benzalkonium chloride within the range of 0.10-10.0μg/L had a linear relationship (r>0.999). The detection limits ranged from 0.03 to 0.06μg/L. The recoveries of three kinds of benzalkonium chloride were 86.7%-111.2%.
CONCLUSIONS
Verified by samples, this method meets the detection limits and has anti-interference abilities of three benzalkonium chloride homologues in surface water and shallow groundwater. Moreover, it was identified that the suspected disrupting chemical of cetyl dimethyl benzyl ammonium chloride is propylene glycol fatty acid ester at m/z 360.323.

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要点

HIGHLIGHTS

(1) The aqueous samples were filtered by 0.22μm membrane and mixed with methanol of the same volume to enhance the uniformity of the benzalkonium chloride in the sample.

(2) The difference in m/z of 0.01 between the target and interfering matrix was identified, eliminating the interference to C16-BAC.

(3) The advantages of sensitivity and resolution are balanced by SIM mode, and the method has a low detection limit and strong anti-jamming ability.

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