Optimisation of distillation as an isolation method for the determination of low methylmercury concentrations in urine samples

Methylmercury (MeHg) speciation in urine requires a robust, reproducible and sensitive technique that enables reliable measurements in limited sample volumes. Conventional MeHg extraction by acid digestion allows for processing of only small amounts of urine digest, making accurate MeHg determinatio...
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Gespeichert in:

Autor*in:	Alilović, Adna [verfasserIn] Živković, Igor [verfasserIn] Horvat, Milena [verfasserIn]

Format:	E-Artikel
Sprache:	Englisch

Erschienen:	2023

Schlagwörter:	Direct distillation Acid digestion Urine Methylmercury Speciation Uncertainty

Übergeordnetes Werk:	Enthalten in: Talanta - Amsterdam [u.a.] : Elsevier Science, 1958, 264
Übergeordnetes Werk:	volume:264

DOI / URN:	10.1016/j.talanta.2023.124765

Katalog-ID:	ELV010507701

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520			\|a Methylmercury (MeHg) speciation in urine requires a robust, reproducible and sensitive technique that enables reliable measurements in limited sample volumes. Conventional MeHg extraction by acid digestion allows for processing of only small amounts of urine digest, making accurate MeHg determination in low-concentration samples virtually impossible. Distillation has been proven as an efficient isolation method with very low detection limits for measuring MeHg in water samples; therefore, in this study, it was optimised for urine samples. Combined with aqueous phase ethylation, purging with nitrogen, preconcentration on Tenax trap, isothermal gas chromatography and cold vapour atomic fluorescence detection, distillation achieved high and repeatable urine spike recoveries of 94% ± 7%. Larger measured aliquot volume led to a significantly lower limit of detection (LOD) for distillation compared with acid digestion (1.1 versus 5.5 pg g−1 urine). Thirty-two general population urine samples were analysed using both methods, and the results were compared. Distillation led to better separation of MeHg from inorganic Hg and the matrix. Good correlation was observed between the results obtained by the two methods for samples with MeHg concentrations above 10 pg g−1 urine (slope = 0.9492, R2 = 0.9879). For samples below this MeHg concentration, distillation was superior, enabling the measurement of MeHg in 9 out of 12 urine samples that were below the LOD of acid digestion. Distillation had significantly lower measurement uncertainty, particularly in the low-concentration samples, where the expanded combined standard uncertainty of the acid digestion method reached as high as 43.2% (k = 2), predominantly owing to poor sample repeatability.
650		4	\|a Direct distillation
650		4	\|a Acid digestion
650		4	\|a Urine
650		4	\|a Methylmercury
650		4	\|a Speciation
650		4	\|a Uncertainty
700	1		\|a Živković, Igor \|e verfasserin \|4 aut
700	1		\|a Horvat, Milena \|e verfasserin \|4 aut
773	0	8	\|i Enthalten in \|t Talanta \|d Amsterdam [u.a.] : Elsevier Science, 1958 \|g 264 \|h Online-Ressource \|w (DE-627)306712571 \|w (DE-600)1500969-5 \|w (DE-576)251938158 \|x 1873-3573 \|7 nnns
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912			\|a GBV_ILN_2027
912			\|a GBV_ILN_2034
912			\|a GBV_ILN_2044
912			\|a GBV_ILN_2048
912			\|a GBV_ILN_2049
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912			\|a GBV_ILN_4334
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936	b	k	\|a 35.00 \|j Chemie: Allgemeines \|q VZ
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publishDate	2023
allfields	10.1016/j.talanta.2023.124765 doi (DE-627)ELV010507701 (ELSEVIER)S0039-9140(23)00516-7 DE-627 ger DE-627 rda eng 540 VZ 35.00 bkl Alilović, Adna verfasserin (orcid)0000-0001-9889-496X aut Optimisation of distillation as an isolation method for the determination of low methylmercury concentrations in urine samples 2023 nicht spezifiziert zzz rdacontent Computermedien c rdamedia Online-Ressource cr rdacarrier Methylmercury (MeHg) speciation in urine requires a robust, reproducible and sensitive technique that enables reliable measurements in limited sample volumes. Conventional MeHg extraction by acid digestion allows for processing of only small amounts of urine digest, making accurate MeHg determination in low-concentration samples virtually impossible. Distillation has been proven as an efficient isolation method with very low detection limits for measuring MeHg in water samples; therefore, in this study, it was optimised for urine samples. Combined with aqueous phase ethylation, purging with nitrogen, preconcentration on Tenax trap, isothermal gas chromatography and cold vapour atomic fluorescence detection, distillation achieved high and repeatable urine spike recoveries of 94% ± 7%. Larger measured aliquot volume led to a significantly lower limit of detection (LOD) for distillation compared with acid digestion (1.1 versus 5.5 pg g−1 urine). Thirty-two general population urine samples were analysed using both methods, and the results were compared. Distillation led to better separation of MeHg from inorganic Hg and the matrix. Good correlation was observed between the results obtained by the two methods for samples with MeHg concentrations above 10 pg g−1 urine (slope = 0.9492, R2 = 0.9879). For samples below this MeHg concentration, distillation was superior, enabling the measurement of MeHg in 9 out of 12 urine samples that were below the LOD of acid digestion. Distillation had significantly lower measurement uncertainty, particularly in the low-concentration samples, where the expanded combined standard uncertainty of the acid digestion method reached as high as 43.2% (k = 2), predominantly owing to poor sample repeatability. Direct distillation Acid digestion Urine Methylmercury Speciation Uncertainty Živković, Igor verfasserin aut Horvat, Milena verfasserin aut Enthalten in Talanta Amsterdam [u.a.] : Elsevier Science, 1958 264 Online-Ressource (DE-627)306712571 (DE-600)1500969-5 (DE-576)251938158 1873-3573 nnns volume:264 GBV_USEFLAG_U SYSFLAG_U GBV_ELV SSG-OLC-PHA GBV_ILN_20 GBV_ILN_22 GBV_ILN_23 GBV_ILN_24 GBV_ILN_31 GBV_ILN_32 GBV_ILN_40 GBV_ILN_60 GBV_ILN_62 GBV_ILN_65 GBV_ILN_69 GBV_ILN_70 GBV_ILN_73 GBV_ILN_74 GBV_ILN_90 GBV_ILN_95 GBV_ILN_100 GBV_ILN_101 GBV_ILN_105 GBV_ILN_110 GBV_ILN_150 GBV_ILN_151 GBV_ILN_187 GBV_ILN_213 GBV_ILN_224 GBV_ILN_230 GBV_ILN_370 GBV_ILN_602 GBV_ILN_702 GBV_ILN_2001 GBV_ILN_2003 GBV_ILN_2004 GBV_ILN_2005 GBV_ILN_2007 GBV_ILN_2008 GBV_ILN_2009 GBV_ILN_2010 GBV_ILN_2011 GBV_ILN_2014 GBV_ILN_2015 GBV_ILN_2020 GBV_ILN_2021 GBV_ILN_2025 GBV_ILN_2026 GBV_ILN_2027 GBV_ILN_2034 GBV_ILN_2044 GBV_ILN_2048 GBV_ILN_2049 GBV_ILN_2050 GBV_ILN_2055 GBV_ILN_2056 GBV_ILN_2059 GBV_ILN_2061 GBV_ILN_2064 GBV_ILN_2088 GBV_ILN_2106 GBV_ILN_2110 GBV_ILN_2111 GBV_ILN_2112 GBV_ILN_2122 GBV_ILN_2129 GBV_ILN_2143 GBV_ILN_2152 GBV_ILN_2153 GBV_ILN_2190 GBV_ILN_2232 GBV_ILN_2336 GBV_ILN_2470 GBV_ILN_2507 GBV_ILN_4035 GBV_ILN_4037 GBV_ILN_4112 GBV_ILN_4125 GBV_ILN_4242 GBV_ILN_4249 GBV_ILN_4251 GBV_ILN_4305 GBV_ILN_4306 GBV_ILN_4307 GBV_ILN_4313 GBV_ILN_4322 GBV_ILN_4323 GBV_ILN_4324 GBV_ILN_4325 GBV_ILN_4326 GBV_ILN_4333 GBV_ILN_4334 GBV_ILN_4338 GBV_ILN_4393 GBV_ILN_4700 35.00 Chemie: Allgemeines VZ AR 264
spelling	10.1016/j.talanta.2023.124765 doi (DE-627)ELV010507701 (ELSEVIER)S0039-9140(23)00516-7 DE-627 ger DE-627 rda eng 540 VZ 35.00 bkl Alilović, Adna verfasserin (orcid)0000-0001-9889-496X aut Optimisation of distillation as an isolation method for the determination of low methylmercury concentrations in urine samples 2023 nicht spezifiziert zzz rdacontent Computermedien c rdamedia Online-Ressource cr rdacarrier Methylmercury (MeHg) speciation in urine requires a robust, reproducible and sensitive technique that enables reliable measurements in limited sample volumes. Conventional MeHg extraction by acid digestion allows for processing of only small amounts of urine digest, making accurate MeHg determination in low-concentration samples virtually impossible. Distillation has been proven as an efficient isolation method with very low detection limits for measuring MeHg in water samples; therefore, in this study, it was optimised for urine samples. Combined with aqueous phase ethylation, purging with nitrogen, preconcentration on Tenax trap, isothermal gas chromatography and cold vapour atomic fluorescence detection, distillation achieved high and repeatable urine spike recoveries of 94% ± 7%. Larger measured aliquot volume led to a significantly lower limit of detection (LOD) for distillation compared with acid digestion (1.1 versus 5.5 pg g−1 urine). Thirty-two general population urine samples were analysed using both methods, and the results were compared. Distillation led to better separation of MeHg from inorganic Hg and the matrix. Good correlation was observed between the results obtained by the two methods for samples with MeHg concentrations above 10 pg g−1 urine (slope = 0.9492, R2 = 0.9879). For samples below this MeHg concentration, distillation was superior, enabling the measurement of MeHg in 9 out of 12 urine samples that were below the LOD of acid digestion. Distillation had significantly lower measurement uncertainty, particularly in the low-concentration samples, where the expanded combined standard uncertainty of the acid digestion method reached as high as 43.2% (k = 2), predominantly owing to poor sample repeatability. Direct distillation Acid digestion Urine Methylmercury Speciation Uncertainty Živković, Igor verfasserin aut Horvat, Milena verfasserin aut Enthalten in Talanta Amsterdam [u.a.] : Elsevier Science, 1958 264 Online-Ressource (DE-627)306712571 (DE-600)1500969-5 (DE-576)251938158 1873-3573 nnns volume:264 GBV_USEFLAG_U SYSFLAG_U GBV_ELV SSG-OLC-PHA GBV_ILN_20 GBV_ILN_22 GBV_ILN_23 GBV_ILN_24 GBV_ILN_31 GBV_ILN_32 GBV_ILN_40 GBV_ILN_60 GBV_ILN_62 GBV_ILN_65 GBV_ILN_69 GBV_ILN_70 GBV_ILN_73 GBV_ILN_74 GBV_ILN_90 GBV_ILN_95 GBV_ILN_100 GBV_ILN_101 GBV_ILN_105 GBV_ILN_110 GBV_ILN_150 GBV_ILN_151 GBV_ILN_187 GBV_ILN_213 GBV_ILN_224 GBV_ILN_230 GBV_ILN_370 GBV_ILN_602 GBV_ILN_702 GBV_ILN_2001 GBV_ILN_2003 GBV_ILN_2004 GBV_ILN_2005 GBV_ILN_2007 GBV_ILN_2008 GBV_ILN_2009 GBV_ILN_2010 GBV_ILN_2011 GBV_ILN_2014 GBV_ILN_2015 GBV_ILN_2020 GBV_ILN_2021 GBV_ILN_2025 GBV_ILN_2026 GBV_ILN_2027 GBV_ILN_2034 GBV_ILN_2044 GBV_ILN_2048 GBV_ILN_2049 GBV_ILN_2050 GBV_ILN_2055 GBV_ILN_2056 GBV_ILN_2059 GBV_ILN_2061 GBV_ILN_2064 GBV_ILN_2088 GBV_ILN_2106 GBV_ILN_2110 GBV_ILN_2111 GBV_ILN_2112 GBV_ILN_2122 GBV_ILN_2129 GBV_ILN_2143 GBV_ILN_2152 GBV_ILN_2153 GBV_ILN_2190 GBV_ILN_2232 GBV_ILN_2336 GBV_ILN_2470 GBV_ILN_2507 GBV_ILN_4035 GBV_ILN_4037 GBV_ILN_4112 GBV_ILN_4125 GBV_ILN_4242 GBV_ILN_4249 GBV_ILN_4251 GBV_ILN_4305 GBV_ILN_4306 GBV_ILN_4307 GBV_ILN_4313 GBV_ILN_4322 GBV_ILN_4323 GBV_ILN_4324 GBV_ILN_4325 GBV_ILN_4326 GBV_ILN_4333 GBV_ILN_4334 GBV_ILN_4338 GBV_ILN_4393 GBV_ILN_4700 35.00 Chemie: Allgemeines VZ AR 264
allfields_unstemmed	10.1016/j.talanta.2023.124765 doi (DE-627)ELV010507701 (ELSEVIER)S0039-9140(23)00516-7 DE-627 ger DE-627 rda eng 540 VZ 35.00 bkl Alilović, Adna verfasserin (orcid)0000-0001-9889-496X aut Optimisation of distillation as an isolation method for the determination of low methylmercury concentrations in urine samples 2023 nicht spezifiziert zzz rdacontent Computermedien c rdamedia Online-Ressource cr rdacarrier Methylmercury (MeHg) speciation in urine requires a robust, reproducible and sensitive technique that enables reliable measurements in limited sample volumes. Conventional MeHg extraction by acid digestion allows for processing of only small amounts of urine digest, making accurate MeHg determination in low-concentration samples virtually impossible. Distillation has been proven as an efficient isolation method with very low detection limits for measuring MeHg in water samples; therefore, in this study, it was optimised for urine samples. Combined with aqueous phase ethylation, purging with nitrogen, preconcentration on Tenax trap, isothermal gas chromatography and cold vapour atomic fluorescence detection, distillation achieved high and repeatable urine spike recoveries of 94% ± 7%. Larger measured aliquot volume led to a significantly lower limit of detection (LOD) for distillation compared with acid digestion (1.1 versus 5.5 pg g−1 urine). Thirty-two general population urine samples were analysed using both methods, and the results were compared. Distillation led to better separation of MeHg from inorganic Hg and the matrix. Good correlation was observed between the results obtained by the two methods for samples with MeHg concentrations above 10 pg g−1 urine (slope = 0.9492, R2 = 0.9879). For samples below this MeHg concentration, distillation was superior, enabling the measurement of MeHg in 9 out of 12 urine samples that were below the LOD of acid digestion. Distillation had significantly lower measurement uncertainty, particularly in the low-concentration samples, where the expanded combined standard uncertainty of the acid digestion method reached as high as 43.2% (k = 2), predominantly owing to poor sample repeatability. Direct distillation Acid digestion Urine Methylmercury Speciation Uncertainty Živković, Igor verfasserin aut Horvat, Milena verfasserin aut Enthalten in Talanta Amsterdam [u.a.] : Elsevier Science, 1958 264 Online-Ressource (DE-627)306712571 (DE-600)1500969-5 (DE-576)251938158 1873-3573 nnns volume:264 GBV_USEFLAG_U SYSFLAG_U GBV_ELV SSG-OLC-PHA GBV_ILN_20 GBV_ILN_22 GBV_ILN_23 GBV_ILN_24 GBV_ILN_31 GBV_ILN_32 GBV_ILN_40 GBV_ILN_60 GBV_ILN_62 GBV_ILN_65 GBV_ILN_69 GBV_ILN_70 GBV_ILN_73 GBV_ILN_74 GBV_ILN_90 GBV_ILN_95 GBV_ILN_100 GBV_ILN_101 GBV_ILN_105 GBV_ILN_110 GBV_ILN_150 GBV_ILN_151 GBV_ILN_187 GBV_ILN_213 GBV_ILN_224 GBV_ILN_230 GBV_ILN_370 GBV_ILN_602 GBV_ILN_702 GBV_ILN_2001 GBV_ILN_2003 GBV_ILN_2004 GBV_ILN_2005 GBV_ILN_2007 GBV_ILN_2008 GBV_ILN_2009 GBV_ILN_2010 GBV_ILN_2011 GBV_ILN_2014 GBV_ILN_2015 GBV_ILN_2020 GBV_ILN_2021 GBV_ILN_2025 GBV_ILN_2026 GBV_ILN_2027 GBV_ILN_2034 GBV_ILN_2044 GBV_ILN_2048 GBV_ILN_2049 GBV_ILN_2050 GBV_ILN_2055 GBV_ILN_2056 GBV_ILN_2059 GBV_ILN_2061 GBV_ILN_2064 GBV_ILN_2088 GBV_ILN_2106 GBV_ILN_2110 GBV_ILN_2111 GBV_ILN_2112 GBV_ILN_2122 GBV_ILN_2129 GBV_ILN_2143 GBV_ILN_2152 GBV_ILN_2153 GBV_ILN_2190 GBV_ILN_2232 GBV_ILN_2336 GBV_ILN_2470 GBV_ILN_2507 GBV_ILN_4035 GBV_ILN_4037 GBV_ILN_4112 GBV_ILN_4125 GBV_ILN_4242 GBV_ILN_4249 GBV_ILN_4251 GBV_ILN_4305 GBV_ILN_4306 GBV_ILN_4307 GBV_ILN_4313 GBV_ILN_4322 GBV_ILN_4323 GBV_ILN_4324 GBV_ILN_4325 GBV_ILN_4326 GBV_ILN_4333 GBV_ILN_4334 GBV_ILN_4338 GBV_ILN_4393 GBV_ILN_4700 35.00 Chemie: Allgemeines VZ AR 264
allfieldsGer	10.1016/j.talanta.2023.124765 doi (DE-627)ELV010507701 (ELSEVIER)S0039-9140(23)00516-7 DE-627 ger DE-627 rda eng 540 VZ 35.00 bkl Alilović, Adna verfasserin (orcid)0000-0001-9889-496X aut Optimisation of distillation as an isolation method for the determination of low methylmercury concentrations in urine samples 2023 nicht spezifiziert zzz rdacontent Computermedien c rdamedia Online-Ressource cr rdacarrier Methylmercury (MeHg) speciation in urine requires a robust, reproducible and sensitive technique that enables reliable measurements in limited sample volumes. Conventional MeHg extraction by acid digestion allows for processing of only small amounts of urine digest, making accurate MeHg determination in low-concentration samples virtually impossible. Distillation has been proven as an efficient isolation method with very low detection limits for measuring MeHg in water samples; therefore, in this study, it was optimised for urine samples. Combined with aqueous phase ethylation, purging with nitrogen, preconcentration on Tenax trap, isothermal gas chromatography and cold vapour atomic fluorescence detection, distillation achieved high and repeatable urine spike recoveries of 94% ± 7%. Larger measured aliquot volume led to a significantly lower limit of detection (LOD) for distillation compared with acid digestion (1.1 versus 5.5 pg g−1 urine). Thirty-two general population urine samples were analysed using both methods, and the results were compared. Distillation led to better separation of MeHg from inorganic Hg and the matrix. Good correlation was observed between the results obtained by the two methods for samples with MeHg concentrations above 10 pg g−1 urine (slope = 0.9492, R2 = 0.9879). For samples below this MeHg concentration, distillation was superior, enabling the measurement of MeHg in 9 out of 12 urine samples that were below the LOD of acid digestion. Distillation had significantly lower measurement uncertainty, particularly in the low-concentration samples, where the expanded combined standard uncertainty of the acid digestion method reached as high as 43.2% (k = 2), predominantly owing to poor sample repeatability. Direct distillation Acid digestion Urine Methylmercury Speciation Uncertainty Živković, Igor verfasserin aut Horvat, Milena verfasserin aut Enthalten in Talanta Amsterdam [u.a.] : Elsevier Science, 1958 264 Online-Ressource (DE-627)306712571 (DE-600)1500969-5 (DE-576)251938158 1873-3573 nnns volume:264 GBV_USEFLAG_U SYSFLAG_U GBV_ELV SSG-OLC-PHA GBV_ILN_20 GBV_ILN_22 GBV_ILN_23 GBV_ILN_24 GBV_ILN_31 GBV_ILN_32 GBV_ILN_40 GBV_ILN_60 GBV_ILN_62 GBV_ILN_65 GBV_ILN_69 GBV_ILN_70 GBV_ILN_73 GBV_ILN_74 GBV_ILN_90 GBV_ILN_95 GBV_ILN_100 GBV_ILN_101 GBV_ILN_105 GBV_ILN_110 GBV_ILN_150 GBV_ILN_151 GBV_ILN_187 GBV_ILN_213 GBV_ILN_224 GBV_ILN_230 GBV_ILN_370 GBV_ILN_602 GBV_ILN_702 GBV_ILN_2001 GBV_ILN_2003 GBV_ILN_2004 GBV_ILN_2005 GBV_ILN_2007 GBV_ILN_2008 GBV_ILN_2009 GBV_ILN_2010 GBV_ILN_2011 GBV_ILN_2014 GBV_ILN_2015 GBV_ILN_2020 GBV_ILN_2021 GBV_ILN_2025 GBV_ILN_2026 GBV_ILN_2027 GBV_ILN_2034 GBV_ILN_2044 GBV_ILN_2048 GBV_ILN_2049 GBV_ILN_2050 GBV_ILN_2055 GBV_ILN_2056 GBV_ILN_2059 GBV_ILN_2061 GBV_ILN_2064 GBV_ILN_2088 GBV_ILN_2106 GBV_ILN_2110 GBV_ILN_2111 GBV_ILN_2112 GBV_ILN_2122 GBV_ILN_2129 GBV_ILN_2143 GBV_ILN_2152 GBV_ILN_2153 GBV_ILN_2190 GBV_ILN_2232 GBV_ILN_2336 GBV_ILN_2470 GBV_ILN_2507 GBV_ILN_4035 GBV_ILN_4037 GBV_ILN_4112 GBV_ILN_4125 GBV_ILN_4242 GBV_ILN_4249 GBV_ILN_4251 GBV_ILN_4305 GBV_ILN_4306 GBV_ILN_4307 GBV_ILN_4313 GBV_ILN_4322 GBV_ILN_4323 GBV_ILN_4324 GBV_ILN_4325 GBV_ILN_4326 GBV_ILN_4333 GBV_ILN_4334 GBV_ILN_4338 GBV_ILN_4393 GBV_ILN_4700 35.00 Chemie: Allgemeines VZ AR 264
allfieldsSound	10.1016/j.talanta.2023.124765 doi (DE-627)ELV010507701 (ELSEVIER)S0039-9140(23)00516-7 DE-627 ger DE-627 rda eng 540 VZ 35.00 bkl Alilović, Adna verfasserin (orcid)0000-0001-9889-496X aut Optimisation of distillation as an isolation method for the determination of low methylmercury concentrations in urine samples 2023 nicht spezifiziert zzz rdacontent Computermedien c rdamedia Online-Ressource cr rdacarrier Methylmercury (MeHg) speciation in urine requires a robust, reproducible and sensitive technique that enables reliable measurements in limited sample volumes. Conventional MeHg extraction by acid digestion allows for processing of only small amounts of urine digest, making accurate MeHg determination in low-concentration samples virtually impossible. Distillation has been proven as an efficient isolation method with very low detection limits for measuring MeHg in water samples; therefore, in this study, it was optimised for urine samples. Combined with aqueous phase ethylation, purging with nitrogen, preconcentration on Tenax trap, isothermal gas chromatography and cold vapour atomic fluorescence detection, distillation achieved high and repeatable urine spike recoveries of 94% ± 7%. Larger measured aliquot volume led to a significantly lower limit of detection (LOD) for distillation compared with acid digestion (1.1 versus 5.5 pg g−1 urine). Thirty-two general population urine samples were analysed using both methods, and the results were compared. Distillation led to better separation of MeHg from inorganic Hg and the matrix. Good correlation was observed between the results obtained by the two methods for samples with MeHg concentrations above 10 pg g−1 urine (slope = 0.9492, R2 = 0.9879). For samples below this MeHg concentration, distillation was superior, enabling the measurement of MeHg in 9 out of 12 urine samples that were below the LOD of acid digestion. Distillation had significantly lower measurement uncertainty, particularly in the low-concentration samples, where the expanded combined standard uncertainty of the acid digestion method reached as high as 43.2% (k = 2), predominantly owing to poor sample repeatability. Direct distillation Acid digestion Urine Methylmercury Speciation Uncertainty Živković, Igor verfasserin aut Horvat, Milena verfasserin aut Enthalten in Talanta Amsterdam [u.a.] : Elsevier Science, 1958 264 Online-Ressource (DE-627)306712571 (DE-600)1500969-5 (DE-576)251938158 1873-3573 nnns volume:264 GBV_USEFLAG_U SYSFLAG_U GBV_ELV SSG-OLC-PHA GBV_ILN_20 GBV_ILN_22 GBV_ILN_23 GBV_ILN_24 GBV_ILN_31 GBV_ILN_32 GBV_ILN_40 GBV_ILN_60 GBV_ILN_62 GBV_ILN_65 GBV_ILN_69 GBV_ILN_70 GBV_ILN_73 GBV_ILN_74 GBV_ILN_90 GBV_ILN_95 GBV_ILN_100 GBV_ILN_101 GBV_ILN_105 GBV_ILN_110 GBV_ILN_150 GBV_ILN_151 GBV_ILN_187 GBV_ILN_213 GBV_ILN_224 GBV_ILN_230 GBV_ILN_370 GBV_ILN_602 GBV_ILN_702 GBV_ILN_2001 GBV_ILN_2003 GBV_ILN_2004 GBV_ILN_2005 GBV_ILN_2007 GBV_ILN_2008 GBV_ILN_2009 GBV_ILN_2010 GBV_ILN_2011 GBV_ILN_2014 GBV_ILN_2015 GBV_ILN_2020 GBV_ILN_2021 GBV_ILN_2025 GBV_ILN_2026 GBV_ILN_2027 GBV_ILN_2034 GBV_ILN_2044 GBV_ILN_2048 GBV_ILN_2049 GBV_ILN_2050 GBV_ILN_2055 GBV_ILN_2056 GBV_ILN_2059 GBV_ILN_2061 GBV_ILN_2064 GBV_ILN_2088 GBV_ILN_2106 GBV_ILN_2110 GBV_ILN_2111 GBV_ILN_2112 GBV_ILN_2122 GBV_ILN_2129 GBV_ILN_2143 GBV_ILN_2152 GBV_ILN_2153 GBV_ILN_2190 GBV_ILN_2232 GBV_ILN_2336 GBV_ILN_2470 GBV_ILN_2507 GBV_ILN_4035 GBV_ILN_4037 GBV_ILN_4112 GBV_ILN_4125 GBV_ILN_4242 GBV_ILN_4249 GBV_ILN_4251 GBV_ILN_4305 GBV_ILN_4306 GBV_ILN_4307 GBV_ILN_4313 GBV_ILN_4322 GBV_ILN_4323 GBV_ILN_4324 GBV_ILN_4325 GBV_ILN_4326 GBV_ILN_4333 GBV_ILN_4334 GBV_ILN_4338 GBV_ILN_4393 GBV_ILN_4700 35.00 Chemie: Allgemeines VZ AR 264
language	English
source	Enthalten in Talanta 264 volume:264
sourceStr	Enthalten in Talanta 264 volume:264
format_phy_str_mv	Article
bklname	Chemie: Allgemeines
institution	findex.gbv.de
topic_facet	Direct distillation Acid digestion Urine Methylmercury Speciation Uncertainty
dewey-raw	540
isfreeaccess_bool	false
container_title	Talanta
authorswithroles_txt_mv	Alilović, Adna @@aut@@ Živković, Igor @@aut@@ Horvat, Milena @@aut@@
publishDateDaySort_date	2023-01-01T00:00:00Z
hierarchy_top_id	306712571
dewey-sort	3540
id	ELV010507701
language_de	englisch
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author	Alilović, Adna
spellingShingle	Alilović, Adna ddc 540 bkl 35.00 misc Direct distillation misc Acid digestion misc Urine misc Methylmercury misc Speciation misc Uncertainty Optimisation of distillation as an isolation method for the determination of low methylmercury concentrations in urine samples
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topic_title	540 VZ 35.00 bkl Optimisation of distillation as an isolation method for the determination of low methylmercury concentrations in urine samples Direct distillation Acid digestion Urine Methylmercury Speciation Uncertainty
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title	Optimisation of distillation as an isolation method for the determination of low methylmercury concentrations in urine samples
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title_full	Optimisation of distillation as an isolation method for the determination of low methylmercury concentrations in urine samples
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title_sort	optimisation of distillation as an isolation method for the determination of low methylmercury concentrations in urine samples
title_auth	Optimisation of distillation as an isolation method for the determination of low methylmercury concentrations in urine samples
abstract	Methylmercury (MeHg) speciation in urine requires a robust, reproducible and sensitive technique that enables reliable measurements in limited sample volumes. Conventional MeHg extraction by acid digestion allows for processing of only small amounts of urine digest, making accurate MeHg determination in low-concentration samples virtually impossible. Distillation has been proven as an efficient isolation method with very low detection limits for measuring MeHg in water samples; therefore, in this study, it was optimised for urine samples. Combined with aqueous phase ethylation, purging with nitrogen, preconcentration on Tenax trap, isothermal gas chromatography and cold vapour atomic fluorescence detection, distillation achieved high and repeatable urine spike recoveries of 94% ± 7%. Larger measured aliquot volume led to a significantly lower limit of detection (LOD) for distillation compared with acid digestion (1.1 versus 5.5 pg g−1 urine). Thirty-two general population urine samples were analysed using both methods, and the results were compared. Distillation led to better separation of MeHg from inorganic Hg and the matrix. Good correlation was observed between the results obtained by the two methods for samples with MeHg concentrations above 10 pg g−1 urine (slope = 0.9492, R2 = 0.9879). For samples below this MeHg concentration, distillation was superior, enabling the measurement of MeHg in 9 out of 12 urine samples that were below the LOD of acid digestion. Distillation had significantly lower measurement uncertainty, particularly in the low-concentration samples, where the expanded combined standard uncertainty of the acid digestion method reached as high as 43.2% (k = 2), predominantly owing to poor sample repeatability.
abstractGer	Methylmercury (MeHg) speciation in urine requires a robust, reproducible and sensitive technique that enables reliable measurements in limited sample volumes. Conventional MeHg extraction by acid digestion allows for processing of only small amounts of urine digest, making accurate MeHg determination in low-concentration samples virtually impossible. Distillation has been proven as an efficient isolation method with very low detection limits for measuring MeHg in water samples; therefore, in this study, it was optimised for urine samples. Combined with aqueous phase ethylation, purging with nitrogen, preconcentration on Tenax trap, isothermal gas chromatography and cold vapour atomic fluorescence detection, distillation achieved high and repeatable urine spike recoveries of 94% ± 7%. Larger measured aliquot volume led to a significantly lower limit of detection (LOD) for distillation compared with acid digestion (1.1 versus 5.5 pg g−1 urine). Thirty-two general population urine samples were analysed using both methods, and the results were compared. Distillation led to better separation of MeHg from inorganic Hg and the matrix. Good correlation was observed between the results obtained by the two methods for samples with MeHg concentrations above 10 pg g−1 urine (slope = 0.9492, R2 = 0.9879). For samples below this MeHg concentration, distillation was superior, enabling the measurement of MeHg in 9 out of 12 urine samples that were below the LOD of acid digestion. Distillation had significantly lower measurement uncertainty, particularly in the low-concentration samples, where the expanded combined standard uncertainty of the acid digestion method reached as high as 43.2% (k = 2), predominantly owing to poor sample repeatability.
abstract_unstemmed	Methylmercury (MeHg) speciation in urine requires a robust, reproducible and sensitive technique that enables reliable measurements in limited sample volumes. Conventional MeHg extraction by acid digestion allows for processing of only small amounts of urine digest, making accurate MeHg determination in low-concentration samples virtually impossible. Distillation has been proven as an efficient isolation method with very low detection limits for measuring MeHg in water samples; therefore, in this study, it was optimised for urine samples. Combined with aqueous phase ethylation, purging with nitrogen, preconcentration on Tenax trap, isothermal gas chromatography and cold vapour atomic fluorescence detection, distillation achieved high and repeatable urine spike recoveries of 94% ± 7%. Larger measured aliquot volume led to a significantly lower limit of detection (LOD) for distillation compared with acid digestion (1.1 versus 5.5 pg g−1 urine). Thirty-two general population urine samples were analysed using both methods, and the results were compared. Distillation led to better separation of MeHg from inorganic Hg and the matrix. Good correlation was observed between the results obtained by the two methods for samples with MeHg concentrations above 10 pg g−1 urine (slope = 0.9492, R2 = 0.9879). For samples below this MeHg concentration, distillation was superior, enabling the measurement of MeHg in 9 out of 12 urine samples that were below the LOD of acid digestion. Distillation had significantly lower measurement uncertainty, particularly in the low-concentration samples, where the expanded combined standard uncertainty of the acid digestion method reached as high as 43.2% (k = 2), predominantly owing to poor sample repeatability.
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title_short	Optimisation of distillation as an isolation method for the determination of low methylmercury concentrations in urine samples
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Optimisation of distillation as an isolation method for the determination of low methylmercury concentrations in urine samples

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