PMID- 29195146 OWN - NLM STAT- MEDLINE DCOM- 20180221 LR - 20180221 IS - 1873-376X (Electronic) IS - 1570-0232 (Linking) VI - 1072 DP - 2018 Jan 1 TI - Fast and quantitative determination of saxitoxin and neosaxitoxin in urine by ultra performance liquid chromatography-triple quadrupole mass spectrometry based on the cleanup of solid phase extraction with hydrophilic interaction mechanism. PG - 267-272 LID - S1570-0232(17)30998-4 [pii] LID - 10.1016/j.jchromb.2017.11.032 [doi] AB - Saxitoxin (STX) and neosaxitoxin (NEO) are water-soluble toxins and their cleanup in bio-matrix is a hot topic but difficult problem. A fast and quantitative determination method for STX and NEO in urine was developed using ultra performance liquid chromatography-triple quadrupole mass spectrometry (LC-MS/MS) based on the cleanup of solid phase extraction (SPE) with hydrophilic interaction (HILIC) mechanism. Acetonitrile/methanol/water mixture was used to extract the toxins in urine. Polyamide (PA) was used as HILIC SPE material to clean the toxins in sample matrix. The limits of detection were 0.2ngmL(-1) for STX and 1ngmL(-1) for NEO in urine. The linear ranges were 0.5ngmL(-1)-99.2ngmL(-1) with the correlation coefficient of r=0.9992 for STX and 2.1ngmL(-1)-207ngmL(-1) with r=0.997 for NEO in urine matrix. The recoveries at three spiking levels were 81.5%-117% with the relative standard deviations (RSDs) of 5.4%-8.5% for STX and 89.0%-118% with the RSDs of 6.7%-9.1% for NEO. STX was found in all the 6 patients' urines while NEO was only found in one sample from an intoxication case. CI - Copyright (c) 2017 Elsevier B.V. All rights reserved. FAU - Xu, Xiao-Min AU - Xu XM AD - Zhejiang Provincial Center for Disease Control and Prevention, Hangzhou, 310051, China. Electronic address: chemxuxm@163.com. FAU - Huang, Bai-Fen AU - Huang BF AD - Zhejiang Provincial Center for Disease Control and Prevention, Hangzhou, 310051, China. FAU - Xu, Jiao-Jiao AU - Xu JJ AD - Zhejiang Provincial Center for Disease Control and Prevention, Hangzhou, 310051, China. FAU - Cai, Zeng-Xuan AU - Cai ZX AD - Zhejiang Provincial Center for Disease Control and Prevention, Hangzhou, 310051, China. FAU - Zhang, Jing AU - Zhang J AD - Zhejiang Provincial Center for Disease Control and Prevention, Hangzhou, 310051, China. FAU - Chen, Qing AU - Chen Q AD - Zhejiang Provincial Center for Disease Control and Prevention, Hangzhou, 310051, China. FAU - Han, Jian-Long AU - Han JL AD - Zhejiang Provincial Center for Disease Control and Prevention, Hangzhou, 310051, China. Electronic address: jlhan@cdc.zj.cn. LA - eng PT - Journal Article DEP - 20171126 PL - Netherlands TA - J Chromatogr B Analyt Technol Biomed Life Sci JT - Journal of chromatography. B, Analytical technologies in the biomedical and life sciences JID - 101139554 RN - 35523-89-8 (Saxitoxin) RN - 6YRL8BWD9H (neosaxitoxin) SB - IM MH - Chromatography, High Pressure Liquid/*methods MH - Humans MH - Hydrophobic and Hydrophilic Interactions MH - Limit of Detection MH - Linear Models MH - Reproducibility of Results MH - Saxitoxin/*analogs & derivatives/chemistry/isolation & purification/*urine MH - Solid Phase Extraction/*methods MH - Tandem Mass Spectrometry/*methods OTO - NOTNLM OT - Hydrophilic interaction OT - Liquid chromatography-triple quadrupole mass spectrometry OT - Neosaxitoxin OT - Saxitoxin OT - Solid phase extraction OT - Urine EDAT- 2017/12/02 06:00 MHDA- 2018/02/22 06:00 CRDT- 2017/12/02 06:00 PHST- 2017/06/01 00:00 [received] PHST- 2017/11/22 00:00 [revised] PHST- 2017/11/24 00:00 [accepted] PHST- 2017/12/02 06:00 [pubmed] PHST- 2018/02/22 06:00 [medline] PHST- 2017/12/02 06:00 [entrez] AID - S1570-0232(17)30998-4 [pii] AID - 10.1016/j.jchromb.2017.11.032 [doi] PST - ppublish SO - J Chromatogr B Analyt Technol Biomed Life Sci. 2018 Jan 1;1072:267-272. doi: 10.1016/j.jchromb.2017.11.032. Epub 2017 Nov 26.