Wei sheng yan jiu = Journal of hygiene research · 2020
[Ultrasonic assisted-dispersive solid-phase extraction for rapid enrichment of N-nitrosodimethylamine in water].
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Zhou Jian, Chen Xiaohong, Jin Micong
Аннотация
OBJECTIVE: a novel and rapid analytical method was established for the extraction of N-nitrosodimethylamine in large-volume water samples.
METHODS: Pretreatment was on the basis of ultrasonic-assisted-dispersed solid phase extraction. Coco housing activated carbon was incorporated into the water samples, and the rapid enrichment of N-nitrosodimethylamine was realized by implementing ultrasonic-assisted dispersion. After that, the suspension was filtered by suction, and the residue was eluted by dichloromethane. The eluate was collected and then concentrated to dry using rotary evaporation. Ultra-high performance liquid chromatography tandem mass spectrometer, which equipped with atmospheric pressure chemical ionization source was employed for determination under the multiple reaction monitoring mode.
RESULTS: Limit of detection and quantification for N-nitrosodimethylamine in 500 mL water was 2. 0 ng/mL and 6. 0 ng/mL, respectively. Throughout the validation, good linearity with R~2>0. 999 were achieved with the range from 0. 5 ng/mL to 150. 0 ng/mL. Satisfactory recovery(95. 7%-100. 8%) and inter-day reproducibility(<4. 2%) were obtained by three-level spiking experiments in different water matrices. Finally, the established method was applied for analysis of 48 real samples, the detectable concentrations of positive samples were in the range of <2. 0 ng/L to 14. 4 ng/L.
CONCLUSION: Compared with the traditional solid-phase extraction method, this method ology showed the characteristics of rapid and more efficient, and could save at least 50% of the pretreatment time. Meanwhile, the result of method ology validation were satisfactory.
METHODS: Pretreatment was on the basis of ultrasonic-assisted-dispersed solid phase extraction. Coco housing activated carbon was incorporated into the water samples, and the rapid enrichment of N-nitrosodimethylamine was realized by implementing ultrasonic-assisted dispersion. After that, the suspension was filtered by suction, and the residue was eluted by dichloromethane. The eluate was collected and then concentrated to dry using rotary evaporation. Ultra-high performance liquid chromatography tandem mass spectrometer, which equipped with atmospheric pressure chemical ionization source was employed for determination under the multiple reaction monitoring mode.
RESULTS: Limit of detection and quantification for N-nitrosodimethylamine in 500 mL water was 2. 0 ng/mL and 6. 0 ng/mL, respectively. Throughout the validation, good linearity with R~2>0. 999 were achieved with the range from 0. 5 ng/mL to 150. 0 ng/mL. Satisfactory recovery(95. 7%-100. 8%) and inter-day reproducibility(<4. 2%) were obtained by three-level spiking experiments in different water matrices. Finally, the established method was applied for analysis of 48 real samples, the detectable concentrations of positive samples were in the range of <2. 0 ng/L to 14. 4 ng/L.
CONCLUSION: Compared with the traditional solid-phase extraction method, this method ology showed the characteristics of rapid and more efficient, and could save at least 50% of the pretreatment time. Meanwhile, the result of method ology validation were satisfactory.