PMID- 36868026 OWN - NLM STAT- MEDLINE DCOM- 20230331 LR - 20230331 IS - 1873-264X (Electronic) IS - 0731-7085 (Linking) VI - 228 DP - 2023 May 10 TI - In-syringe dispersive solid phase filter extraction cleanup followed by liquid chromatography-triple quadrupole mass spectrometry for fast determination of colchicine in plasma/urine. PG - 115317 LID - S0731-7085(23)00086-9 [pii] LID - 10.1016/j.jpba.2023.115317 [doi] AB - As an effective treatment for acute gouty arthritis and cardiovascular disease, colchicine is also a toxic alkaloid and may cause poisoning or even death in overdose. The study of colchicine elimination and the diagnosis of poisoning etiology need the rapid and accurate quantitative analysis method in biological matrix. An analytical method was developed for colchicine in plasma and urine by in-syringe dispersive solid phase extraction (DSPE) followed by liquid chromatography-triple quadrupole mass spectrometry (LC-MS/MS). Sample extraction and protein precipitation were proceeded with acetonitrile. The extract was cleaned by in-syringe DSPE. An XBridge BEH C(18) column(100 mm x 2.1 mm, 2.5 microm)was used to separate colchicine by gradient elution with mobile phase of 0.01% (v/v) ammonia-methanol. The amount and filling sequence of magnesium sulfate (MgSO(4)) and primary secondary amine (PSA) suitable for in-syringe DSPE were studied. Scopolamine was screened as the quantitative internal standard (IS) for colchicine analysis according to the consistency of recovery rate, chromatographic retention time and matrix effects. The limits of detection for colchicine in plasma and urine were both 0.06 ng mL(-1) and the limits of quantitation were both 0.2 ng mL(-1). The linear range was 0.04 - 20 ng mL(-1) (Equivalent to 0.2-100 ng mL(-1) in plasma or urine) with a correlation coefficient r > 0.999. By IS calibration, the average recoveries at three spiking levels in plasma and urine were 95.3-102.68% and 93.9-94.8% with the relative standard deviations (RSDs) of 2.9-5.7% and 2.3-3.4%, respectively. The matrix effects, stability, dilution effects and carryover for determination of colchicine in plasma and urine were also evaluated. The elimination of colchicine within 72-384 h post-ingestion was studied for a poisoning patient with the doses of 1 mg d(-1) for 39 days and then 3 mg d(-1) for 15 days). CI - Copyright (c) 2023 Elsevier B.V. All rights reserved. FAU - Qian, Ming-Rong AU - Qian MR AD - key Laboratory of Pollution Exposure and Health Intervention of Zhejiang Province, Interdisciplinary Research Academy, Zhejiang Shuren University, Hangzhou 310015, China. FAU - Chen, Zhi-Min AU - Chen ZM AD - Lishui Bluetown Agricultural Testing Technology Co., Ltd., Lishui 323000, China. FAU - Tao, Xue-Xin AU - Tao XX AD - key Laboratory of Pollution Exposure and Health Intervention of Zhejiang Province, Interdisciplinary Research Academy, Zhejiang Shuren University, Hangzhou 310015, China. FAU - Yao, Feng AU - Yao F AD - Department of Emergency Medicine, the First Affiliated Hospital, School of Medicine, Zhejiang University, Hangzhou 310003, China. FAU - Xu, Xiao-Min AU - Xu XM AD - Zhejiang Provincial Center for Disease Control and Prevention, Hangzhou 310051, China. Electronic address: chemxuxm@163.com. LA - eng PT - Journal Article DEP - 20230227 PL - England TA - J Pharm Biomed Anal JT - Journal of pharmaceutical and biomedical analysis JID - 8309336 RN - SML2Y3J35T (Colchicine) SB - IM MH - Humans MH - Chromatography, Liquid/methods MH - *Colchicine MH - *Tandem Mass Spectrometry/methods MH - Syringes MH - Solid Phase Extraction MH - Chromatography, High Pressure Liquid/methods OTO - NOTNLM OT - Colchicine OT - Drug elimination OT - In-syringe dispersive solid phase extraction OT - Intoxication OT - Liquid chromatography OT - Triple quadrupole mass spectrometry 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. Declaration of interest We declare that we have no financial and personal relationships with other people or organizations that can inappropriately influence our work. EDAT- 2023/03/04 06:00 MHDA- 2023/03/31 06:42 CRDT- 2023/03/03 18:12 PHST- 2023/01/11 00:00 [received] PHST- 2023/02/17 00:00 [revised] PHST- 2023/02/23 00:00 [accepted] PHST- 2023/03/31 06:42 [medline] PHST- 2023/03/04 06:00 [pubmed] PHST- 2023/03/03 18:12 [entrez] AID - S0731-7085(23)00086-9 [pii] AID - 10.1016/j.jpba.2023.115317 [doi] PST - ppublish SO - J Pharm Biomed Anal. 2023 May 10;228:115317. doi: 10.1016/j.jpba.2023.115317. Epub 2023 Feb 27.