PMID- 35872539 OWN - NLM STAT- MEDLINE DCOM- 20220816 LR - 20220816 IS - 1873-3778 (Electronic) IS - 0021-9673 (Linking) VI - 1678 DP - 2022 Aug 16 TI - Development of magnetic molecularly imprinted solid-phase extraction and ultra-high performance liquid chromatography tandem mass spectrometry for rapid and selective determination of urinary diphenyl phosphate of college students. PG - 463344 LID - S0021-9673(22)00537-4 [pii] LID - 10.1016/j.chroma.2022.463344 [doi] AB - Organophosphate esters (OPEs), known as novel alternative flame retardants, are a class of environmental endocrine disruptors. Long-term exposure to OPEs may bring a non-negligible health risk to human. Urinary OPE metabolites (mOPEs) are generally used as biomarkers to evaluate the internal exposure to OPEs. Diphenyl phosphate (DPHP), the main metabolite of aryl-OPEs, exhibited high detection rates and concentrations in urine samples. To establish a selective and simple analytical method for biomonitoring urinary DPHP, a specific magnetic molecular imprinted polymer (MMIP) was fabricated via a sol-gel method. Under optimum magnetic solid-phase extraction (MSPE) conditions, the resultant MMIP exhibited selective recognition ability, ideal adsorption capacity and good reusability on urinary DPHP enrichment. The developed MSPE method coupled with ultra-high performance liquid chromatography tandem mass spectrometry (U-HPLC-MS/MS) exhibited good precision and accuracy (spiked recoveries of 85.8%-109% with relative standard deviations (RSDs) ranged from 5.1%-13%), low detection limit of 0.035 ng/mL, and negligible matrix inhibition. Then we used this proposed method to detect urinary DPHP levels of recruited 30 college students and investigate the time variability and potential determinants. All urine samples revealed the presence of DPHP at a median concentration of 0.56 mug/g Creatinine (Cr). Moderate reproducibility of DPHP level was observed in first morning urine samples (ICC>0.40). Significant correlations were found between urinary DPHP levels and gender (beta=0.72; 95% CI: 0.48 approximately 0.96), sampling time (beta=0.36; 95% CI: 0.08 approximately 0.65) as well as the frequency for take-out food (beta=0.45; 95% CI: 0.07 approximately 0.74) (p< 0.05). Hence, a fast and sensitive MSPE-U-HPLC-MS/MS method was successfully built to quantify urinary DPHP. CI - Copyright (c) 2022 Elsevier B.V. All rights reserved. FAU - Yu, Meng AU - Yu M AD - State Key Laboratory of Environment Health (Incubation), Key Laboratory of Environment and Health, Ministry of Education, Key Laboratory of Environment and Health (Wuhan), Ministry of Environmental Protection, School of Public Health, Tongji Medical College, Huazhong University of Science and Technology, #13 Hangkong Road, Wuhan, Hubei, 430030, China. FAU - Kou, Jing AU - Kou J AD - State Key Laboratory of Environment Health (Incubation), Key Laboratory of Environment and Health, Ministry of Education, Key Laboratory of Environment and Health (Wuhan), Ministry of Environmental Protection, School of Public Health, Tongji Medical College, Huazhong University of Science and Technology, #13 Hangkong Road, Wuhan, Hubei, 430030, China. FAU - Xu, Qitong AU - Xu Q AD - State Key Laboratory of Environment Health (Incubation), Key Laboratory of Environment and Health, Ministry of Education, Key Laboratory of Environment and Health (Wuhan), Ministry of Environmental Protection, School of Public Health, Tongji Medical College, Huazhong University of Science and Technology, #13 Hangkong Road, Wuhan, Hubei, 430030, China. FAU - Feng, Jingwen AU - Feng J AD - Department of Educational Administration, Guangzhou University of Chinese Medicine, Guangzhou, Guangdong, 510006, China. FAU - Li, Xiang AU - Li X AD - State Key Laboratory of Environment Health (Incubation), Key Laboratory of Environment and Health, Ministry of Education, Key Laboratory of Environment and Health (Wuhan), Ministry of Environmental Protection, School of Public Health, Tongji Medical College, Huazhong University of Science and Technology, #13 Hangkong Road, Wuhan, Hubei, 430030, China. FAU - Zheng, Zhiyi AU - Zheng Z AD - State Key Laboratory of Environment Health (Incubation), Key Laboratory of Environment and Health, Ministry of Education, Key Laboratory of Environment and Health (Wuhan), Ministry of Environmental Protection, School of Public Health, Tongji Medical College, Huazhong University of Science and Technology, #13 Hangkong Road, Wuhan, Hubei, 430030, China. FAU - Liu, Jun AU - Liu J AD - State Key Laboratory of Environment Health (Incubation), Key Laboratory of Environment and Health, Ministry of Education, Key Laboratory of Environment and Health (Wuhan), Ministry of Environmental Protection, School of Public Health, Tongji Medical College, Huazhong University of Science and Technology, #13 Hangkong Road, Wuhan, Hubei, 430030, China. FAU - Mei, Surong AU - Mei S AD - State Key Laboratory of Environment Health (Incubation), Key Laboratory of Environment and Health, Ministry of Education, Key Laboratory of Environment and Health (Wuhan), Ministry of Environmental Protection, School of Public Health, Tongji Medical College, Huazhong University of Science and Technology, #13 Hangkong Road, Wuhan, Hubei, 430030, China. Electronic address: surongmei@hust.edu.cn. LA - eng PT - Journal Article DEP - 20220714 PL - Netherlands TA - J Chromatogr A JT - Journal of chromatography. A JID - 9318488 RN - 0 (Biphenyl Compounds) RN - 0 (Flame Retardants) RN - 0 (Organophosphates) RN - 0 (Phosphates) RN - 2L9GJK6MGN (diphenyl) SB - IM MH - Biphenyl Compounds MH - Chromatography, High Pressure Liquid/methods MH - *Flame Retardants/analysis MH - Humans MH - Magnetic Phenomena MH - Organophosphates/urine MH - Phosphates MH - Reproducibility of Results MH - Solid Phase Extraction MH - Students MH - *Tandem Mass Spectrometry/methods OTO - NOTNLM OT - College students OT - Diphenyl phosphate OT - Magnetic molecularly imprinted solid-phase extraction OT - Organophosphate esters OT - Urine samples COIS- Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper. EDAT- 2022/07/26 06:00 MHDA- 2022/08/17 06:00 CRDT- 2022/07/25 02:23 PHST- 2022/04/29 00:00 [received] PHST- 2022/06/28 00:00 [revised] PHST- 2022/07/13 00:00 [accepted] PHST- 2022/07/26 06:00 [pubmed] PHST- 2022/08/17 06:00 [medline] PHST- 2022/07/25 02:23 [entrez] AID - S0021-9673(22)00537-4 [pii] AID - 10.1016/j.chroma.2022.463344 [doi] PST - ppublish SO - J Chromatogr A. 2022 Aug 16;1678:463344. doi: 10.1016/j.chroma.2022.463344. Epub 2022 Jul 14.