PMID- 31891992 OWN - NLM STAT- MEDLINE DCOM- 20200608 LR - 20200608 IS - 1873-3573 (Electronic) IS - 0039-9140 (Linking) VI - 209 DP - 2020 Mar 1 TI - Application of dispersive liquid-liquid microextraction based on solidification of floating organic drop for the determination of extractables from pharmaceutical packaging materials. PG - 120540 LID - S0039-9140(19)31173-7 [pii] LID - 10.1016/j.talanta.2019.120540 [doi] AB - A new method was established for the determination of the extractables from pharmaceutical packaging materials using dispersive liquid-liquid microextraction based on solidification of floating organic drop (DLLME-SFO) coupled with ultra-high-performance liquid chromatography quadrupole time-of-flight mass spectrometry (UHPLC-QTOF MS). Packaging samples were filled with three kinds of buffer solutions: acid buffer (pH = 3), alkaline buffer (pH = 9) and 0.9% NaCl solution to extract as many extractables as possible, and then the extractables in buffer solutions were enriched by DLLME-SFO technique. Parameters affecting the efficiency of the extraction procedure were evaluated and optimized, including the type and volume of dispersant, extractant volume, pH and vortex-mixing time. After optimization, the values obtained for limits of detection and quantification for three kinds of common antioxidants were 0.3 and 1.0 mug/L respectively, and good linearity (R(2) > 0.99) was observed in their respective concentration ranges. The recoveries ranged from 80.61% to 117.87% at three spiked levels with the relative standard deviations (RSDs) between 0.92% and 9.29% (n = 6) in all three buffer solutions. The developed method was successfully applied to the analysis of extractables from pharmaceutical packaging materials. The results indicated that the proposed procedure is a novel, sensitive, fast and repeatable method and has a great significance for evaluation of safety of pharmaceutical packaging materials. CI - Copyright (c) 2019 Elsevier B.V. All rights reserved. FAU - Sun, Xuechun AU - Sun X AD - College of Chemistry, Beijing University of Chemical Technology, Beijing, 100029, China. FAU - Xing, Xuebin AU - Xing X AD - College of Chemistry, Beijing University of Chemical Technology, Beijing, 100029, China. FAU - Du, Zhenxia AU - Du Z AD - College of Chemistry, Beijing University of Chemical Technology, Beijing, 100029, China; College of Chemistry, Beijing Key Laboratory of Environmentally Harmful Chemical Analysis, Beijing University of Chemical Technology, Beijing, 100029, China. Electronic address: duzx@mail.buct.edu.cn. LA - eng PT - Journal Article DEP - 20191109 PL - Netherlands TA - Talanta JT - Talanta JID - 2984816R RN - 0 (Antioxidants) RN - 0 (Solvents) RN - 0 (Triazoles) RN - 1P9D0Z171K (Butylated Hydroxytoluene) RN - 3896-11-5 (tinuvin) SB - IM MH - Antioxidants/*analysis MH - Butylated Hydroxytoluene/analogs & derivatives/*analysis MH - Chromatography, High Pressure Liquid/methods MH - *Drug Packaging/methods MH - Liquid Phase Microextraction/*methods MH - Mass Spectrometry/methods MH - Solvents MH - Triazoles/*analysis OTO - NOTNLM OT - DLLME-SFO OT - Pharmaceutical packaging materials OT - Safety analysis OT - UHPLC-QTOF MS EDAT- 2020/01/02 06:00 MHDA- 2020/06/09 06:00 CRDT- 2020/01/02 06:00 PHST- 2019/06/19 00:00 [received] PHST- 2019/10/26 00:00 [revised] PHST- 2019/11/03 00:00 [accepted] PHST- 2020/01/02 06:00 [entrez] PHST- 2020/01/02 06:00 [pubmed] PHST- 2020/06/09 06:00 [medline] AID - S0039-9140(19)31173-7 [pii] AID - 10.1016/j.talanta.2019.120540 [doi] PST - ppublish SO - Talanta. 2020 Mar 1;209:120540. doi: 10.1016/j.talanta.2019.120540. Epub 2019 Nov 9.