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New LC-MS/MS method for the determination of eight nitrosamines in drinking water
Date issued
2016
Abstract
"A new sensitive, selective and accurate LC-MS/MS method with positive electrospray
ionization was developed to detect eight nitrosamines from drinking water. The method separates
all nitrosamines using a Zorbax Eclipse Plus C18 column (100 × 2.1 mm, 3.5 µm) kept at 15°C
and a mobile phase consisting of aq. 0.005% formic acid and acetonitrile in the ratio 90/10 (v/v). A
strong gradient applied in 8 min up to 90% ACN allowed analyte separation. A low mobile phase
flw-rate of 0.2 ml/min was used to enhance ESI ionisation. Collision energy, fragmentor and capillary voltages were optimised to enhance analyte S/N ratio. Optimisation of LC-MS parameters
generated low instrumental LOQ values between 0.05–1.84 µg/l. Detector response was linear in
the range 1–100 µg/l (R2 > 0.99) for all nitrosamines. SPE using activated charcoal cartridges was
used to concentrate nitrosamines from drinking water. Overall method LOQs were situated in the
range 1.23–4.12 ng/l. LC-MS/MS method was fully validated with respect to specificity, linearity,
precision, accuracy and LOQ, and provided good results. The method was tested on six tap water
samples collected from different regions of Bucharest and the determined nitrosamine total content
ranged between 2.8 and 14.8 ng/l."
ionization was developed to detect eight nitrosamines from drinking water. The method separates
all nitrosamines using a Zorbax Eclipse Plus C18 column (100 × 2.1 mm, 3.5 µm) kept at 15°C
and a mobile phase consisting of aq. 0.005% formic acid and acetonitrile in the ratio 90/10 (v/v). A
strong gradient applied in 8 min up to 90% ACN allowed analyte separation. A low mobile phase
flw-rate of 0.2 ml/min was used to enhance ESI ionisation. Collision energy, fragmentor and capillary voltages were optimised to enhance analyte S/N ratio. Optimisation of LC-MS parameters
generated low instrumental LOQ values between 0.05–1.84 µg/l. Detector response was linear in
the range 1–100 µg/l (R2 > 0.99) for all nitrosamines. SPE using activated charcoal cartridges was
used to concentrate nitrosamines from drinking water. Overall method LOQs were situated in the
range 1.23–4.12 ng/l. LC-MS/MS method was fully validated with respect to specificity, linearity,
precision, accuracy and LOQ, and provided good results. The method was tested on six tap water
samples collected from different regions of Bucharest and the determined nitrosamine total content
ranged between 2.8 and 14.8 ng/l."
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Nitrozamine JEPE 2016.pdf
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