References for Biomonitoring Analytical Methods

Zhang Y, Wang Q, Zhang G, Jia W, Ren Y, Wu Y. Biomarker analysis of hemoglobin adducts of acrylamide and glycidamide enantiomers for mid-term internal exposure assessment by isotope dilution ultra-high-performance liquid chromatography tandem mass spectrometry. Talanta. 2018;178:825-33.
Duke TJ, Ruestow PS, Marsh GM. The influence of demographic, physical, behavioral, and dietary factors on hemoglobin adduct levels of acrylamide and glycidamide in the general U.S. population. Crit Rev Food Sci Nutr. 2018;58:700-10. doi: 10.1080/10408398.2016.1215289. Epub 2017 Sep 28.
Guo J, Yu D, Lv N, Bai R, Xu C, Chen G, et al. Relationships between acrylamide and glycidamide hemoglobin adduct levels and allergy-related outcomes in general US population, NHANES 2005-2006. Environ Pollut. 2017;225:506-13. doi: 10.1016/j.envpol.2017.03.016. Epub 2017 Mar 18.
Hielscher J, Monien BH, Abraham K, Jessel S, Seidel A, Lampen A. An isotope-dilution UPLC-MS/MS technique for the human biomonitoring of the internal exposure to glycidol via a valine adduct at the N-terminus of hemoglobin. J Chromatogr B Analyt Technol Biomed Life Sci. 2017;1059:7-13.
Yang M, Frame T, Tse C, Vesper HW. High-throughput, simultaneous quantitation of hemoglobin adducts of acrylamide, glycidamide, and ethylene oxide using UHPLC-MS/MS. J Chromatogr B Analyt Technol Biomed Life Sci. 2018 Jun 1;1086:197-205. doi: 10.1016/j.jchromb.2018.03.048. Epub 2018 Apr 3.
Guo J, Yu D, Lv N, Bai R, Xu C, Chen G, et al. Relationships between acrylamide and glycidamide hemoglobin adduct levels and allergy-related outcomes in general US population, NHANES 2005-2006. Environ Pollut. 2017 Jun;225:506-513. doi: 10.1016/j.envpol.2017.03.016. Epub 2017 Mar 18.
Chu PL, Lin LY, Chen PC, Su TC, Lin CY. Negative association between acrylamide exposure and body composition in adults: NHANES, 2003-2004. Nutr Diabetes. 2017 Mar 13;7(3):e246. doi: 10.1038/nutd.2016.48.
Obón-Santacana M, Lujan-Barroso L, Freisling H, Cadeau C, Fagherazzi G, Boutron-Ruault MC, et al. Dietary and lifestyle determinants of acrylamide and glycidamide hemoglobin adducts in non-smoking postmenopausal women from the EPIC cohort. Eur J Nutr. 2017 Apr;56(3):1157-1168. doi: 10.1007/s00394-016-1165-5. Epub 2016 Feb 5.
Obón-Santacana M, Freisling H, Peeters PH, Lujan-Barroso L, Ferrari P, Boutron-Ruault MC, et al. Acrylamide and glycidamide hemoglobin adduct levels and endometrial cancer risk: A nested case-control study in nonsmoking postmenopausal women from the EPIC cohort. Int J Cancer. 2016 Mar 1;138(5):1129-38. doi: 10.1002/ijc.29853. Epub 2015 Oct 1.
Obón-Santacana M, Lujan-Barroso L, Travis RC, Freisling H, Ferrari P, Severi G, et al. Acrylamide and Glycidamide Hemoglobin Adducts and Epithelial Ovarian Cancer: A Nested Case-Control Study in Nonsmoking Postmenopausal Women from the EPIC Cohort. Cancer Epidemiol Biomarkers Prev. 2016 Jan;25(1):127-34. doi: 10.1158/1055-9965.EPI-15-0822. Epub 2015 Nov 23.
Xie J, Terry KL, Poole EM, Wilson KM, Rosner BA, Willett WC, et al. Acrylamide hemoglobin adduct levels and ovarian cancer risk: a nested case-control study. Cancer Epidemiol Biomarkers Prev. 2013 Apr;22(4):653-60. doi: 10.1158/1055-9965.EPI-12-1387. Epub 2013 Feb 15.
Vesper HW, Sternberg MR, Frame T, Pfeiffer CM. Among 10 sociodemographic and lifestyle variables, smoking is strongly associated with biomarkers of acrylamide exposure in a representative sample of the U.S. Population. J Nutr. 2013 Jun;143(6):995S-1000S. doi: 10.3945/jn.112.173013. Epub 2013 Apr 17.
Moorman WJ, Reutman SS, Shaw PB, Blade LM, Marlow D, Vesper H, et al. Occupational exposure to acrylamide in closed system production plants: air levels and biomonitoring. J Toxicol Environ Health A. 2012;75(2):100-11. doi: 10.1080/15287394.2011.615109.
Vesper HW, Caudill SP, Osterloh JD, Meyers T, Scott D, Myers GL. Exposure of the U.S. population to acrylamide in the National Health and Nutrition Examination Survey 2003-2004. Environ Health Perspect. 2010 Feb;118(2):278-83. doi: 10.1289/ehp.0901021.
Tran NL, Barraj LM, Murphy MM, Bi X. Dietary acrylamide exposure and hemoglobin adducts–National Health and Nutrition Examination Survey (2003-04). Food and chemical toxicology: an international journal published for the British Industrial Biological Research Association. 2010;48:3098-108. doi: 10.1016/j.fct.2010.08.003. Epub 2010 Aug 7.
von Stedingk H, Vikstrom AC, Rydberg P, Pedersen M, Nielsen JK, Segerback D, et al. Analysis of hemoglobin adducts from acrylamide, glycidamide, and ethylene oxide in paired mother/cord blood samples from Denmark. Chem Res Toxicol. 2011;24:1957-65.
von Stedingk H, Rydberg P, Tornqvist M. A new modified Edman procedure for analysis of N-terminal valine adducts in hemoglobin by LC-MS/MS. J Chromatogr B Analyt Technol Biomed Life Sci. 2010;878:2483-90.
Schettgen T, Muller J, Fromme H, Angerer J. Simultaneous quantification of haemoglobin adducts of ethylene oxide, propylene oxide, acrylonitrile, acrylamide and glycidamide in human blood by isotope-dilution GC/NCI-MS/MS. J Chromatogr B Analyt Technol Biomed Life Sci. 2010;878:2467-73.
Wilson KM, Vesper HW, Tocco P, Sampson L, Rosén J, Hellenäs KE, et al. Validation of a food frequency questionnaire measurement of dietary acrylamide intake using hemoglobin adducts of acrylamide and glycidamide. Cancer Causes Control. 2009 Apr;20(3):269-78. doi: 10.1007/s10552-008-9241-7. Epub 2008 Oct 15.
Vesper HW, Slimani N, Hallmans G, Tjønneland A, Agudo A, Benetou V, et al. Cross-sectional study on acrylamide hemoglobin adducts in subpopulations from the European Prospective Investigation into Cancer and Nutrition (EPIC) Study. J Agric Food Chem. 2008 Aug 13;56(15):6046-53. doi: 10.1021/jf703750t. Epub 2008 Jul 15.
Vesper HW, Slimani N, Hallmans G, Tjonneland A, Agudo A, Benetou V, et al. Cross-sectional study on acrylamide hemoglobin adducts in subpopulations from the European Prospective Investigation into Cancer and Nutrition (EPIC) study. J Agric Food Chem 2008; 56 (15):6046–53.
Vesper HW, Bernert JT, Ospina M, Meyers T, Ingham L, Smith A, et al. Assessment of the relation between biomarkers for smoking and biomarkers for acrylamide exposure in humans. Cancer Epidemiol Biomarkers Prev 2007;16(11):2471-8.
Vesper HW, Bernert JT, Ospina M, Meyers T, Ingham L, Smith A, et al. Cancer Epidemiol Biomarkers Prev. 2007 Nov;16(11):2471-8. Assessment of the relation between biomarkers for smoking and biomarkers for acrylamide exposure in humans.
Vesper HW, Ospina M, Meyers T, Ingham L, Smith A, Gray JG, et al. Automated method for measuring globin adducts of acrylamide and glycidamide at optimized Edman reaction conditions. Rapid Commun Mass Spectrom. 2006;20(6):959-64.
Ahn HS, Shin HS. Determination of ethylene oxide-hemoglobin adduct by silylation and gas chromatography-electron impact-mass spectrometry. J Chromatogr B Analyt Technol Biomed Life Sci. 2006;843:202-8.
Ospina M, Vesper HW, Licea-Perez H, Meyers T, Mi L, Myers G. LC/MS/MS method for the analysis of acrylamide and glycidamide hemoglobin adducts. Adv Exp Med Biol. 2005;561:97-107.
Vesper HW, Licea-Perez H, Meyers T, Ospina M, Myers GL. Pilot study on the impact of potato chips consumption on biomarkers of acrylamide exposure. Adv Exp Med Biol. 2005;561:89-96.
Ball L, Jones A, Boogaard P, Will W, Aston P. Development of a competitive immunoassay for the determination of N-(2-hydroxyethyl)valine adducts in human haemoglobin and its application in biological monitoring. Biomarkers. 2004;9:407-17.
Schettgen T, Broding HC, Angerer J, Drexler H. Hemoglobin adducts of ethylene oxide, propylene oxide, acrylonitrile and acrylamide-biomarkers in occupational and environmental medicine. Toxicol Lett. 2002;134:65-70.
Boogaard PJ. Use of haemoglobin adducts in exposure monitoring and risk assessment. J Chromatogr B Analyt Technol Biomed Life Sci. 2002;778:309-22.
Thier R, Lewalter J, Kempkes M, Selinski S, Bruning T, Bolt HM. Haemoglobin adducts of acrylonitrile and ethylene oxide in acrylonitrile workers, dependent on polymorphisms of the glutathione transferases GSTT1 and GSTM1. Arch Toxicol. 1999;73:197-202.
Boogaard PJ, Rocchi PS, van Sittert NJ. Biomonitoring of exposure to ethylene oxide and propylene oxide by determination of hemoglobin adducts: correlations between airborne exposure and adduct levels. Int Arch Occup Environ Health. 1999;72:142-50.
Bono R, Vincenti M, Meineri V, Pignata C, Saglia U, Giachino O, et al. Formation of N-(2-hydroxyethyl)valine due to exposure to ethylene oxide via tobacco smoke: A risk factor for onset of cancer. Environ Res. 1999;81:62-71.
Bergmark E. Hemoglobin adducts of acrylamide and acrylonitrile in laboratory workers, smokers and nonsmokers. Chem Res Toxicol. 1997;10:78-84.
Tavares R, Borba H, Monteiro M, Proenca MJ, Lynce N, Rueff J, et al. Monitoring of exposure to acrylonitrile by determination of N-(2-cyanoethyl)valine at the N-terminal position of haemoglobin. Carcinogenesis. 1996;17:2655-60.
Lawrence RM, Sweetman GM, Tavares R, Farmer PB. Synthesis and characterization of peptide adducts for use in monitoring human exposure to acrylonitrile and ethylene oxide. Teratog Carcinog Mutagen. 1996;16:139-48.

Yu LL, Caceres GC, Long SE, Murphy KE, Bryan Sallee CE, Vetter TW, C. Hagwood, M.A. Franklin, J. Castro Georgi, J. M. Jarrett, D.M. Jones, R.L. Jones, Z. Li, Y.L. Sommer, D. S. Tevis, K. Wallon, C.D. Ward, M. Maras, S. Erdahl, C. Gilmer, M. Wermers, H. Woldeysus, K.F. Mehigan, M. Morrissette, C.D. Palmer and P.J. Parsons, “Certification of Standard Reference Material® 955d Toxic Elements and Metabolites in Frozen Human Blood “, 2020, NIST, https://doi.org/10.6028/NIST.SP.260-206external icon.
Tevisexternal icon DS, Jarrett JM,external icon Jones DR, external icon Cheng PY, external icon Franklin M, external icon Mullinex N, external icon Caldwell KL, external iconand Jonesexternal icon RL, “Assessing the stability of Cd, Mn, Pb, Se, and total Hg in whole human blood by ICP-DRC-MS as a function of temperature and time“, Clinica Chimica Acta.
Jones, D.R., et al. “Biomonitoring method for measurement of As, Cr, and Ni in human urine samples by ICP-UCT-MS.” International Journal of Hygiene and Environmental Health. Volume 234, May 2021, 113713. [NHANES 2017-2020]
Sommer YL, Ward CD, Castro Georgi J, Cheng PY, Jones RL. “Importance of Preanalytical Factors in Measuring Cr and Co Levels in Human Whole Blood: Contamination Control, Proper Sample Collection and Long-Term Storage Stability.” J Anal Toxicol, 2021;45(3): 297–307. [NHANES 2011-current]
Castro Georgi J, YL, Ward CD, Cheng PY, Jones RL and Caldwell KL, “Biomonitoring method for the analysis of chromium and cobalt in human whole blood using inductively coupled plasma-kinetic energy discrimination-mass spectrometry (ICP-KED-MS)“, Anal. Methods, 2017, 9 (23), 3464-3476. [NHANES 2015-2020]
Jones DR, Jarrett JM, Tevis DS, Franklin M, Mullinix NJ, Wallon KL, et al. Analysis of whole human blood for Pb, Cd, Hg, Se, and Mn by ICP-DRC-MS for biomonitoring and acute exposures. Talanta 2017;162: 114-22. [NHANES 2003-2018]
Quarles CD Jr, Jones DR, Jarrett JM, Shakirova G, Pan Y, Caldwell KL, et al. Analytical method for total chromium and nickel in urine using an inductively coupled plasma-universal cell technology-mass spectrometer (ICP-UCT-MS) in kinetic energy discrimination (KED) mode. J Anal At Spectrom 2014;29(2): 297-303. [NHANES 2017-current]
Sommer YL, Verdon CP, Fresquez MR, Ward CD, Wood EB, Pan Y, et al. Measurement of mercury species in human blood using triple spike isotope dilution with SPME-GC-ICP-DRCMS. Anal Bioanal Chem 2014;406(20):5039-47. [NHANES 2011-current]
Ruha, A. M., et al., (2009). “Urine mercury excretion following meso-dimercaptosuccinic acid challenge in fish eaters.” Archives of Pathology and Laboratory Medicine 133(1): 87-92.[NHANES 2003-2020]
Jarrett JM, Xiao G, Caldwell K, Henahan D, Shakirova G, Jones RL. Eliminating molybdenum oxide interference in urine cadmium biomonitoring using ICP-DRC-MS. J Anal At Spectrom 2008;23(7): 962-967. [NHANES 1999–current]
Verdon CP, Caldwell KL, Fresques MR, Jones RL. Determination of seven arsenic compounds in urine by HPLC-ICP-DRC-MS: a CDC population biomonitoring method. Anal Bioanal Chem 2008;393(3):939-947. [NHANES 2003-current]
Jarrett JM, Jones RL, Caldwell KL, Verdon CP. Total urine arsenic measurements using inductively coupled plasma mass spectrometry with a dynamic reaction cell. At Spectrosc 2007;28(4):113-22. [NHANES 2003-2016]
Albalak R, Jones RL, Caldwell KL, Miller G. Inorganic mercury determination in whole blood using on-line microwave digestion with flow injection mercury system (FIMS). At Spectrosc 2005;26(6): 234-40. [NHANES 1999 –¬ 2010]
Caldwell KL, Hartel J, Jarrett J, Jones RL. Inductively coupled plasma mass spectrometry to measure multiple toxic elements in urine in NHANES 1999-2000. At Spectrosc 2005;26(1):1-7. [NHANES 1999-current]
Caldwell, K. L., et al., (2003). “Use of Inductively Coupled Plasma Mass Spectrometry to Measure Urinary Iodine in NHANES 2000: Comparison with Previous Method.” Clinical Chemistry 49(6): 1019-1021. [NHANES 1999-2020]
Chen HP, Paschal DC, Miller DT, Morrow JC. Determination of total and inorganic mercury in whole blood by on-line digestion with flow injection. Atomic Spectroscopy 1998;19:176-179.
Guo, T. and J. Baasner (1993). “On-line microwave sample pretreatment for the determination of mercury in blood by flow injection cold vapor atomic absorption spectrometry.” Talanta (Oxford) 40(12): 1927-36. [NHANES 1999 – 2002]
Parsons, P, Slavin W. A rapid Zeeman graphite furnace atomic absorption spectrometric method for the determination of lead in blood. Spectrochimica acta. Part B, At Spectrosc 1993;48(6-7): 925-39.[NHANES 1999 – 2002]
Miller DT, Paschal DC, Gunter EW, Stroud PE, D’Angelo J. Determination of blood lead with electrothermal atomic absorption using a L’vov platform and matrix modifier. Analyst 1987;112:1701-4. [NHANES III – 2002]
Paschal DC, Kimberly MM. Automated direct determination of selenium in serum by electrothermal atomic absorption spectroscopy. At Spectrosc 1986;7:75-8. [NHANES III]
Lewis, S. A., Hardison, N. W., & Veillon, C. Comparison of isotope dilution mass spectrometry and graphite furnace atomic absorption spectrometry with Zeeman background correction for the determination of plasma selenium. Anal Chem 1986;58(6): 1272-3. [NHANES III]
Pruszkowska E, Carnrick GR, Slavin W. Direct determination of cadmium in urine with use of a stabilized temperature platform furnace and Zeeman background correction. Clin Chem 1983;29:477-80. [NHANES III]
Stoeppler M, Brandt K. Determination of cadmium in whole blood and urine by electrothermal atomic-absorption spectrophotometry. Fresnius A Anal Chem 1980;300:372-380.[NHANES 1999 – 2002]
Barthel, W. F., et al., (1973). “Modified Delves cup atomic absorption determination of lead in blood.” Journal – Association of Official Analytical Chemists 56(5): 1252-1256. [NHANES II]Sommer YL, Ward CD, Pan Y, Caldwell KL, and Jones RL. “Long-Term Stability of Inorganic, Methyl, and Ethyl Mercury in Whole Blood: Effects of Storage Temperature and Time.” J Anal Toxicol, 2016;40(3): 222-228. [NHANES 2011-current]

Parker DL, Rybak ME, Pfeiffer CM. Phytoestrogen biomonitoring: an extractionless LC-MS/MS method for measuring urinary isoflavones and lignans by use of atmospheric pressure photoionization (APPI). Anal Bioanal Chem 2012;402:1123-1136. (NHANES 2005-2006 and later)
Rybak ME, Parker DL, Pfeiffer CM. Determination of urinary phytoestrogens by HPLC–MS/MS: A comparison of atmospheric pressure chemical ionization (APCI) and electrospray ionization (ESI). J Chromatogr R 2008;861:145-150. (NHANES 2003-2004)
Kuklenyik Z, Ye X, Reich JA, Needham LL, Calafat AM. Automated on-line and off-line solid phase extraction methods for measuring isoflavones and lignans in urine. J Chromatogr Sci 2004; 42:495-500.
Valentin-Blasini L, Blount BC, Rogers HS, Needham LL. HPLC-MS/MS method for the measurement of seven phytoestrogens in human serum and urine. J Expo Anal Environ Epidemiol 2000;10:799-807.

Bravo R, Caltabiano LM, Fernandez C, Smith KD, Gallegos M, Whitehead RD, et al. Quantification of phenolic metabolites of environmental chemicals in human urine using gas chromatography-tandem mass spectrometry and isotope dilution quantification. J Chromatog B 2005;820(2):229-236.
Hill RH Jr, Shealy DB, Head SL, Williams CC, Bailey SL, Gregg M, et al. Determination of pesticide metabolites in human urine using isotope dilution technique and tandem mass spectrometry. J Anal Toxicol 1995;19(5):323-329.

Montesano MA, Olsson AO, Kuklenyik P, Needham LL, Bradman AS, Barr DB. Method for determination of acephate, methamidophos, omethoate, dimethoate, ethylenethiourea and propylenethiourea in human urine using high-performance liquid chromatography-atmospheric pressure chemical ionization tandem mass spectrometry. J Expo Sci Environ Epidemiol. 2007;17(4):321-30.
Bravo R, Caltabiano LM, Fernandez C, Smith KD, Gallegos M, Whitehead RD, et al. Quantification of phenolic metabolites of environmental chemicals in human urine using gas chromatography-tandem mass spectrometry and isotope dilution quantification. J Chromatog B 2005;820(2):229-236.
Ye X, Kuklenyik Z, Needham LL, Calafat AM. Automated on-line column-switching HPLCMS/MS method with peak focusing for the determination of nine environmental phenols in urine. Anal Chem 2005;77:5407-13.

2,4-D and 2,4,5-T

Davis MD, Wade EL, Restrepo PR, Roman-Esteva W, Bravo R, Kuklenyik P, et al. Semiautomated solid phase extraction method for the mass spectrometric quantification of 12 specific metabolites of organophosphorus pesticides, synthetic pyrethroids, and select herbicides in human urine. J Chromatogr B 2013;929:18-26. (NHANES 2007-2008 and later)
Olsson AO, Baker SE, Nguyen JV, Romanoff LC, Udunka SO, Walker RD, et al. A liquid chromatography-tandem mass spectrometry multiresidue method for quantification of specific metabolites of organophosphorus pesticides, synthetic pyrethroids, selected herbicides, and DEET in human urine. Anal Chem 2004;76(9):2453-61. (NHANES 1999-2004)

Atrazine

Kuklenyik Z, Panuwet P, Jayatilaka NK, Pirkle JL, Calafat AM. Two-dimensional high performance liquid chromatography separation and tandem mass spectrometry detection of atrazine and its metabolic and hydrolysis products in urine. J Chromatogr B Analyt Technol Biomed Life Sci. 2012 Jul 15;901:1-8.

Glyphosate

Schütze A, Morales-Agudelo P, Vidal M, Calafat AM, Ospina M. Quantification of glyphosate and other organophosphorus compounds in human urine via ion chromatography isotope dilution tandem mass spectrometry. Chemosphere. 2021 Jul;274:129427. doi: 10.1016/j.chemosphere.2020.129427. Epub 2021 Jan 12. PMID: 33529959.

Sulfonylurea Herbicides

Nguyen JV, Olsson AO, Bravo R, Needham LL, Barr DB. Quantification of atrazine, phenylurea, and sulfonylurea herbicide metabolites in urine by high-performance liquid chromatographytandem mass spectrometry. J Anal Toxicol. 2007;31(4):181-6.
Baker SE, Olsson AO, Needham LL, Barr DB. High-performance liquid chromatography-tandem mass spectrometry method for quantifying sulfonylurea herbicides in human urine: reconsidering the validation process. Anal Bioanal Chem 2005; 383:963-76.

Kuklenyik P, Baker SE, Bishop AM, Morales-A P, Calafat AM. On-line solid phase extraction-high performance liquid chromatography-isotope dilution-tandem mass spectrometry approach to quantify N,N-diethyl-m-toluamide and oxidative metabolites in urine. Anal Chim Acta. 2013 Jul 17;787:267-73. (For NHANES 2007-2008 through 2013-2014)
Baker SE, Bishop-Serafim A, Morales-Agudelo P, Vidal M, Ospina M, and Calafat AM. “Quantification of DEET and Neonicotinoid Pesticide Biomarkers in Human Urine by Online Solid Phase Extraction-High Performance Liquid Chromatography-Tandem Mass Spectrometry” Anal. Bional Chem. (2019) 411:669–678 https://doi.org/10.1007/s00216-018-1481-0 (For NHANES 2015-16)

Baker SE, Bishop-Serafim A, Morales-Agudelo P, Vidal M, Ospina M, and Calafat AM. “Quantification of DEET and Neonicotinoid Pesticide Biomarkers in Human Urine by Online Solid Phase Extraction-High Performance Liquid Chromatography-Tandem Mass Spectrometry” Anal. Bional Chem. (2019) 411:669–678 https://doi.org/10.1007/s00216-018-1481-0 (For NHANES 2015-16).

Bravo R, Caltabiano LM, Weerasekera G, Whitehead RD, Fernandez C, Needham LL, et al. Measurement of dialkyl phosphate metabolites of organophosphorus pesticides in human urine using lyophilization with gas chromatography-tandem mass spectrometry and isotope dilution quantification. J Expo Anal Environ Epidemiol 2004;14:249-259.
Bravo R, Driskell WJ, Whitehead RD Jr, Needham LL, Barr DB. Quantitation of dialkyl phosphate metabolites of organophosphate pesticides in human urine using GC-MS-MS with isotopic internal standards. J Anal Toxicol 2002;26:245-252.
Jayatilaka NK, Restrepo P, Davis Z, Vidal M, Calafat AM, Ospina M. “Quantification of 16 urinary biomarkers of exposure to flame retardants, plasticizers, and organophosphate insecticides for biomonitoring studies” Chemosphere. 2019 Jun 26;235:481-491. doi: 10.1016/j.chemosphere.2019.06.181. [Epub ahead of print] (For NHANES 2011-2012 and 2015-2016).

Davis MD, Wade EL, Restrepo PR, Roman-Esteva W, Bravo R, Kuklenyik P, et al. Semiautomated solid phase extraction method for the mass spectrometric quantification of 12 specific metabolites of organophosphorus pesticides, synthetic pyrethroids, and select herbicides in human urine. J Chromatogr B 2013;929:18-26. (NHANES 2007-2008 and later)
Montesano MA, Olsson AO, Kuklenyik P, Needham LL, Bradman AS, Barr DB. Method for determination of acephate, methamidophos, omethoate, dimethoate, ethylenethiourea and propylenethiourea in human urine using high-performance liquid chromatography-atmospheric pressure chemical ionization tandem mass spectrometry. J Expo Sci Environ Epidemiol. 2007;17(4):321-30.
Olsson AO, Baker SE, Nguyen JV, Romanoff LC, Udunka SO, Walker RD, et al. A liquid chromatography-tandem mass spectrometry multiresidue method for quantification of specific metabolites of organophosphorus pesticides, synthetic pyrethroids, selected herbicides, and DEET in human urine. Anal Chem 2004;76(9):2453-61. (NHANES 1999-2004)

Ye X, Kuklenyik Z, Bishop AM, Needham LL, Calafat AM. Quantification of the urinary concentrations of parabens in humans by on-line solid phase extraction-high performance liquid chromatography isotope dilution tandem mass spectrometry. J Chromatogr B 2006;844:53-9.
Ye X, Kuklenyik Z, Needham LL, Calafat AM. Automated on-line column-switching HPLCMS/MS method with peak focusing for the determination of nine environmental phenols in urine. Anal Chem 2005;77:5407-13.

Patterson, DG Jr., Wong L-Y, Turner WE, Caudill SP, DiPietro ES, McClure PC, et al. Levels in the U.S. population of those persistent organic pollutants (2003-2004) included in the Stockholm Convention or in other Long-Range Transboundary Air Pollution Agreements. Environ Sci Technol 2009;43(4):1211-8.
Jones R, Edenfield E, Anderson S, Zhang Y and Sjodin A. Semi-automated extraction and cleanup method for measuring persistent organic pollutants in human serum. Organohalogen Compounds 2012;74:97-8.
Sjodin A, Jones RS, Lapeza CR, Focant JF, McGahee EE III, Patterson DG. Semiautomated high-throughput extraction and cleanup method for the measurement of polybrominated diphenyl ethers, polybrominated biphenyls, and polychlorinated biphenyls in human serum. Anal Chem 2004;76:1921-7.
Patterson DG Jr., Alexander LR, Turner WE, Isaacs SG, Needham LL. The development and application of a high resolution mass spectrometry method for measuring polychlorinated dibenzo-p-dioxins and dibenzofurans in serum. In: Clement RE, Sui KM, Hill HH Jr., eds. Instrumentation for trace organic monitoring. Chelsea, MI: Lewis Publishers; 1990. pp. 119-53.
Patterson DG Jr., Hampton L, Lapeza CR Jr., Belser WT, Green V, Alexander L, et al. High resolution gas chromatographic/high resolution mass spectrometric analysis of human serum on a whole weight and lipid basis for 2,3,7,8 TCDD. Anal Chem 1987;59:2000-5.

Kato K, Kalathil AA, Patel AM, Ye X, Calafat AM. Per- and polyfluoroalkyl substances and fluorinated alternatives in urine and serum by on-line solid phase extraction-liquid chromatography-tandem mass spectrometry. Chemosphere. 2018 Oct;209:338-345. (For NHANES 2013-14 in urine; from NHANES 2015+ in serum)
Kato K, Basden BJ, Needham LL, Calafat AM. Improved selectivity for the analysis of maternal serum and cord serum for polyfluoroalkyl chemicals. J Chromatogr A 2011;1218(15):2133-2137.
Kuklenyik Z, Needham LL, Calafat AM. Measurement of 18 perfluorinated organic acids and amides in human serum using on-line solid-phase extraction. Anal Chem 2005;77:6085-6091.
Kuklenyik Z, Reich JA, Tully JS, Needham LL, Calafat AM. Automated solid-phase extraction and measurement of perfluorinated organic acids and amides in human serum and milk. Environ Sci Technol. 2004 Jul 1;38(13):3698-704.

Zhou X, Kramer JP, Calafat AM, Ye X. Automated on-line column-switching high performance liquid chromatography isotope dilution tandem mass spectrometry method for the quantification of bisphenol A, bisphenol F, bisphenol S, and 11 other phenols in urine. J Chromatogr B Analyt Technol Biomed Life Sci. 2014 Jan 1;944:152-6.
Dwivedi P, Zhou X, Powell TG, Calafat AM, Ye X. Impact of enzymatic hydrolysis on the quantification of total urinary concentrations of chemical biomarkers. Chemosphere. 2018 May;199:256-262.
Ye X, Kuklenyik Z, Bishop AM, Needham LL, Calafat AM. Quantification of the urinary concentrations of parabens in humans by on-line solid phase extraction-high performance liquid chromatography isotope dilution tandem mass spectrometry. J Chromatogr B 2006;844:53-9.
Ye X, Kuklenyik Z, Needham LL, Calafat AM. Automated on-line column-switching HPLCMS/MS method with peak focusing for the determination of nine environmental phenols in urine. Anal Chem 2005;77:5407-13.

Silva MJ, Wong LY, Samandar E, Preau JL, Calafat AM, Ye X. Exposure to di-2-ethylhexyl terephthalate in a convenience sample of U.S. adults from 2000 to 2016. Arch Toxicol. 2017 Oct;91(10):3287-3291. Erratum to: Exposure to di-2-ethylhexyl terephthalate in a convenience sample of U.S. adults from 2000 to 2016. Silva MJ, Wong LY, Samandar E, Preau JL, Calafat AM, Ye X. Arch Toxicol. 2017 Oct;91(10):3293. (from NHANES 2015+)
Silva MJ, Jia T, Samandar E, Preau JL, Calafat AM. Environmental exposure to plasticizer 1,2- cyclohexane dicarboxylic acid, diisononyl ester (DINCH) in US adults (2000-2012). Environ Res 2013; 126: 159-163. (NHANES 2011-2014)
Silva MJ, Samandar E, Preau JL, Reidy JA, Needham LL, Calafat AM. Quantification of 22 phthalate metabolites in human urine. J Chromatogr B 2007;860:106-12. (NHANES 2005-2012)
Kato K, Silva MJ, Needham LL, Calafat AM. Determination of 16 phthalate metabolites in urine using automated sample preparation and on-line preconcentration/high-performance liquid chromatography/tandem mass spectrometry. Anal Chem 2005;77(9):2985-91. (NHANES 2003- 2004)
Silva MJ, Slakman AR, Reidy JA, Preau JLJ, Herbert AR, Samandar E, et al. Analysis of human urine for 15 phthalate metabolites using automated solid-phase extraction. J Chromatogr B 2004;805:161-7. (NHANES 2001-2002)
Silva MJ, Malek NA, Hodge CC, Reidy JA, Kato K, Barr DB, et al. Improved quantitative detection of 11 urinary phthalate metabolites in humans using liquid chromatography atmospheric pressure chemical ionization tandem mass spectrometry. J Chromatogr B 2003;789:393-404. (NHANES 1999-2000)
Blount BC, Milgram KE, Silva M, Malek N, Reidy J, Needham LL, et al. Quantitative detection of eight phthalate metabolites in human urine using HPLC-APCI-MS/MS. Anal Chem 2000;72:4127-4134.

Jones R, Edenfield E, Anderson S, Zhang Y, Sjodin A. Semi-automated extraction and cleanup method for measuring persistent organic pollutants in human serum. Organohalogen Compounds 2012;74: 97-8.
Sjodin A, Jones RS, Lapeza CR, Focant JF, McGahee EE III, Patterson DG. Semiautomated high-throughput extraction and cleanup method for the measurement of polybrominated diphenyl ethers, polybrominated biphenyls, and polychlorinated biphenyls in human serum. Anal Chem 2004;76:1921-7.

Turner WE, Whitfield WE, Cash TP, DiPietro ES, Anderson CJ, McClure PC, et al. Same sample cleanup for PCDDs/PCDFs/cPCBs, PCNs and PBDDs/PBDFs in human serum and quantification by GC/ID-HRMS. Organohalogen Compounds 2011; 73: 661-4.
Patterson, DG Jr., Wong L-Y, Turner WE, Caudill SP, DiPietro ES, McClure PC, et al. Levels in the U.S. population of those persistent organic pollutants (2003-2004) included in the Stockholm Convention or in other Long-Range Transboundary Air Pollution Agreements. Environ Sci Technol 2009;43(4):1211-8.
Patterson DG Jr., Alexander LR, Turner WE, Isaacs SG, Needham LL. The development and application of a high resolution mass spectrometry method for measuring polychlorinated dibenzo-p-dioxins and dibenzofurans in serum. In: Clement RE, Sui KM, Hill HH Jr., eds. Instrumentation for Trace Organic Monitoring. Chelsea, MI: Lewis Publishers; 1990. pp. 119-53.
Turner WE, DiPietro E, Cash TP, McClure PC, Patterson DG Jr., Shirkhan H. An improved SPE extraction and automated sample cleanup method for serum PCDDs, PCDFs, and coplanar PCBs. Organohalogen Compounds 1994; 19: 31-5.
Patterson DG Jr., Hampton L, Lapeza CR Jr., Belser WT, Green V, Alexander L, et al. High resolution gas chromatographic/high resolution mass spectrometric analysis of human serum on a whole weight and lipid basis for 2,3,7,8 TCDD. Anal Chem 1987;59: 2000-5.

Wang Y, Meng L, Pittman EN, Etheredge A, Hubbard K, Trinidad DA, et al. Quantification of urinary mono-hydroxylated metabolites of polycyclic aromatic hydrocarbons by on-line solid phase extraction-high performance liquid chromatography-tandem mass spectrometry. Anal Bioanal Chem. 2017 Feb;409(4):931-937. (NHANES 2013-2014)
Li Z, Romanoff LC, Trinidad DA, Hussain N, Jones RS, Porter EN, et al. Measurement of urinary Monohydroxy polycyclic aromatic hydrocarbons using automated liquid-liquid extraction and gas chromatography/isotope dilution high-resolution mass spectrometry. Anal Chem 2006;78:5744-51.
Romanoff LC, Li Z, Young KJ, Blakely NC III, Patterson DG, Sandau CD. Automated solid-phase extraction method for measuring urinary polycyclic aromatic hydrocarbon metabolites in human biomonitoring using isotope-dilution gas chromatography high-resolution mass spectrometry. J Chromatog B 2006;835:47-54.
Smith CJ, Huang WL, Walcott CJ, Turner WE, Grainger J, Patterson DG Jr. Quantification of monohydroxy-PAH metabolites in urine by solid-phase extraction with isotope dilution GC-HRMS. Anal Bioanal Chem 2002;372:216-220.

Davis MD, Wade EL, Restrepo PR, Roman-Esteva W, Bravo R, Kuklenyik P, Calafat AM. Semiautomated solid phase extraction method for the mass spectrometric quantification of 12 specific metabolites of organophosphorus pesticides, synthetic pyrethroids, and select herbicides in human urine. J Chromatogr B 2013;929:18-26. (NHANES 2007-2008 and later)
Olsson AO, Baker SE, Nguyen JV, Romanoff LC, Udunka SO, Walker RD, et al. A liquid chromatography-tandem mass spectrometry multiresidue method for quantification of specific metabolites of organophosphorus pesticides, synthetic pyrethroids, selected herbicides, and DEET in human urine. Anal Chem 2004;76(9):2453-2461.

Jayatilaka NK, Restrepo P, Williams L, Ospina M, Valentin-Blasini L, Calafat AM. Quantification of three chlorinated dialkyl phosphates, diphenyl phosphate, 2,3,4,5-tetrabromobenzoic acid, and four other organophosphates in human urine by solid phase extraction-high performance liquid chromatography-tandem mass spectrometry. Anal Bioanal Chem. (2017) 409:1323–1332. (For NHANES 2013-14)
Jayatilaka NK, Restrepo P, Davis Z, Vidal M, Calafat AM, Ospina M. “Quantification of 16 urinary biomarkers of exposure to flame retardants, plasticizers, and organophosphate insecticides for biomonitoring studies” Chemosphere. 2019 Jun 26;235:481-491. doi: 10.1016/j.chemosphere.2019.06.181. [Epub ahead of print] (NHANES 2011-12, 15-16)

Zhang L, Xia Y, Xia B, Nicodemus KJ, McGuffey J, McGahee E, et al. High-throughput and sensitive analysis of urinary heterocyclic aromatic amines using isotope-dilution liquid chromatography-tandem mass spectrometry and robotic sample preparation system. Anal Bioanal Chem. 2016 Nov;408(28):8149-8161.

Silva LK, Hile GA, Capella KM, Espenship MF, Smith MM, De Jesús VR, Blount BC. Quantification of 19 Aldehydes in Human Serum by Headspace SPME/GC/High-Resolution Mass Spectrometry. Environ Sci Technol 2018;52 (18):10571-10579.

NNAL and Tobacco-specific Nitrosamines (TSNAs; TEBL)

Xia Y, McGuffey JE, Bhattacharyya S, Sellergren B, Yilmaz E, Wang L, et al. Analysis of the tobacco-specific nitrosamine 4-(methylnitrosamino)-1-(3-pyridyl)-1-butanol in urine by extraction on a molecularly imprinted polymer column and liquid chromatography/atmospheric pressure ionization tandem mass spectrometry. Anal Chem. 2005;77(23):7639-45.
Xia Y, Bernert JT. Stability of the tobacco-specific nitrosamine 4-(methylnitrosamino)-1-(3- pyridyl)-1-butanol (NNAL) in urine samples stored at various temperatures. J Anal Toxicol 2010:34:411-5.
Xia B, Xia Y, Wong J, Nicodemus KJ, Xu M, Lee J, et al. Quantitative analysis of five tobacco-specific N-nitrosamines in urine by liquid chromatography-atmospheric pressure ionization tandem mass spectrometry. Biomed Chromatogr. 2014;28(3):375-384.
Xia B, Blount BC, Guillot T, Brosius C, Li Y, Van Bemmel DM, et al. Tobacco-Specific Nitrosamines (NNAL, NNN, NAT, and NAB) Exposures in the US Population Assessment of Tobacco and Health (PATH) Study Wave 1 (2013-2014). Nicotine Tob Res. 2021 Feb 16;23(3):573-583.

Serum Cotinine and Hydroxycotinine (TEBL)

Bernert JT, Turner WE, Pirkle JL, Sosnoff CS, Akins JR, Waldrep MK, et al. Development and validation of sensitive method for determination of serum cotinine in smokers and nonsmokers by liquid chromatography/atmospheric pressure ionization tandem mass spectrometry. Clin Chem 1997;43:2281-91.
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Pirkle JL, Bernert JT, Caudill SP, Sosnoff CS, Pechacek TF. Trends in the exposure of nonsmokers in the U.S. population to secondhand smoke: 1988-2002. Environ Health Perspect. 2006;114(6):853-858.
Bernert JT, Jacob P 3rd, Holiday DB, Benowitz NL, Sosnoff CS, Doig MV, et al. Interlaboratory comparability of serum cotinine measurements at smoker and nonsmoker concentration levels: a round-robin study. Nicotine Tob Res. 2009 Dec;11(12):1458-66.

Urinary Tobacco Alkaloids and Metabolites (TEBL)

Bernert JT, Harmon TL, Sosnoff CS, McGuffey JE. Use of cotinine immunoassay test strips for preclassifying urine samples from smokers and nonsmokers prior to analysis by LC-MS-MS. J Anal Toxicol 2005;29:814-818
McGuffey JE, Wei B, Bernert JT, Morrow JC, Xia B, Wang L, Blount BC. Validation of a LC-MS/MS method for quantifying urinary nicotine, six nicotine metabolites and the minor tobacco alkaloids–anatabine and anabasine–in smokers’ urine. PLoS One. 2014 Jul 11;9(7).
Wei B, Feng J, Rehmani IJ, Miller S, McGuffey JE, Blount BC, Wang L. A high-throughput robotic sample preparation system and HPLC-MS/MS for measuring urinary anatabine, anabasine, nicotine and major nicotine metabolites. Clin Chim Acta. 2014 Sep 25;436:290-7.
Wang L, Bernert JT, Benowitz NL, Feng J, Jacob P 3rd, McGahee E, et al. Collaborative Method Performance Study of the Measurement of Nicotine, Its Metabolites, and Total Nicotine Equivalents in Human Urine. Cancer Epidemiol Biomarkers Prev. 2018 Sep;27(9):1083-1090.
Achilihu, H., Feng, J., Wang L., and Bernert, J. T., Tobacco Use Classification by Inexpensive Urinary Cotinine Immunoassay Test Strips. J Anal Toxicol, 2019. 43(2): p. 149-153.

Seyler TH, Bernert JT. Analysis of 4-aminobiphenyl in smoker’s and nonsmoker’s urine by tandem mass spectrometry. 2011 May;16(3):212-21.
Mazumder S, Ahamed RA, McGahee E, Wang L, Seyler TH. A New Automated Method for the Analysis of Aromatic Amines in Human Urine by GC-MS/MS. ˗J Anal Toxicol. 2019 Jan 1;43(1):25-35.

Bhandari D, Ruhl J, Murphy A, McGahee E, Chambers D, Blount B. Isotope Dilution UPLC-APCI-MS/MS Method for the Quantitative Measurement of Aromatic Diamines in Human Urine: Biomarkers of Diisocyanates Exposure Anal Chem 2016; 88:

Seyler TH, Kim JG, Hodgson JA, Cowan EA, Blount BC, Wang L. Quantitation of urinary volatile nitrosamines from exposure to tobacco smoke. J Anal Toxicol. 2013 May;37(4):195-202.
Hodgson JA, Seyler TH, McGahee E, Arnstein S, Wang L. A New Automated Method and Sample Data Flow for Analysis of Volatile Nitrosamines in Human Urine. Am J Analyt Chem. 2016 Feb;7(2):165-178.
Hodgson JA, Seyler TH, Wang L. Long-Term Stability of Volatile Nitrosamines in Human Urine. J Anal Toxicol. 2016 Jul;40(6):414-8.

Chambers DM, Ocariz JM, McGuirk MF, Bount BC. Impact of cigarette smoking on volatile organic compound (VOC) blood levels in the U.S. Population: NHANES 2003–2004. Environ. Int. 2011;37:1321-8.
Alwis KU, Blount BC, Silva LK, Smith MM, Loose KH. Method for quantifying nitromethane in blood as a potential biomarker of halonitromethane exposure. Environ Sci Technol 2008;42 (7): 2522-7.
Chambers DM, Blount BC, McElprang DO, Waterhouse MG, Morrow J. Picogram measurement of volatile n-alkanes (n-hexane through n-dodecane) in blood using solid-phase microextraction to assess nonoccupational petroleum-based fuel exposure. Anal Chem 2008;80(12): 4666-74.
Chambers DM, McElprang DO, Waterhouse MG, Blount BC. An improved approach for accurate quantitation of benzene, toluene, ethylbenzene, xylene, and styrene in blood. Anal Chem 2006;78 (15): 5375-83.
Blount BC, Kobelski RJ, McElprang DO, Ashley DL, Morrow JC, Chambers DM, et al. Quantification of 31 volatile organic compounds in whole blood using solid-phase microextraction and gas chromatography-mass spectrometry. J Chromatogr B Analyt Technol Biomed Life Sci 2006;832: 292-301.
Bonin MA, Silva LK, Smith MM, Ashley DL, Blount BC. Measurement of trihalomethanes and methyl tert-butyl ether in whole blood using gas chromatography with high-resolution mass spectrometry. J Anal Toxicol 2005;29(2):81-9.
Chambers DM, McElprang DO, Mauldin JP, Hughes TM, Blount BC. Identification and elimination of polysiloxane curing agent interference encountered in the quantification of low picogram per milliliter methyl tert-butyl ether in blood by solid-phase microextraction headspace analysis. Anal Chem 2005;77 (9): 2912-9.

Bhandari, D., McCarthy, D., Biren, C., Movassaghi, C., Blount, B. C., & De Jesús, V. R. (2019). Development of a UPLC-ESI-MS/MS method to measure urinary metabolites of selected VOCs: Benzene, cyanide, furfural, furfuryl alcohol, 5-hydroxymethylfurfural, and N-methyl-2-pyrrolidone. Journal of Chromatography B, 1126, 121746.
Alwis KU, Bailey TL, Patel D, Wang L, Blount BC. Measuring urinary N-acetyl-S-(4-hydroxy-2-methyl-2-buten-1-yl)-L-cysteine (IPMA3) as a potential biomarker of isoprene exposure. Anal Chim Acta 2016;941:61-66.
Alwis KU, Blount BC, Britt AS, Patel D, Ashley DL. Simultaneous analysis of 28 urinary VOC metabolites using ultra high performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry (UPLC-ESI/MSMS). Anal Chim Acta 2012;750:152-60.

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Page last reviewed: March 24, 2022

Content source: Centers for Disease Control and Prevention