JOURNAL OF CHROMATOGRAPHY A
·
2019
·
IF 3.858
Jia Chen,Wenwen Deng,Xiao Li,Xuanxuan Wang,Yuxiu Xiao
A novel supramolecular solvent (SUPRAS) based on hexafluoroisopropanol (HFIP)/Brij-35 was proposed for liquid-phase microextraction (LPME) of parabens in water samples, pharmaceuticals and personal care products. Brij-35 is a cost-effective and non-toxic non-ionic surfactant, but it has a high cloud point (>100 °C). HFIP, with the features of strong hydrogen-bond donor, high density and powerful hydrophobicity, was used as the cloud point-reducing agent and self-assembling and density-regulating solvent of Brij-35. Upon adding HFIP into the Brij-35 aqueous solution, the cloud point of Brij-35 was decreased to below room temperature, and the SUPRAS was formed in the bottom over a wide range of HFIP and Brij-35 concentrations at room temperature. The SUPRAS was composed of Brij-35, HFIP and water, having a density larger than water, and it showed a large spherical structure of positive micellar aggregates (2–8 μm). The HFIP/ Brij-35 SUPRAS-based LPME procedure was non-thermodependent and could be performed at room temperature with centrifugation using normal centrifuge tubes, being very simple. In the extraction of six parabens, the HFIP/ Brij-35 SUPRAS-based LPME method showed short extraction time (3.3 min), low solvent consumption (0.3 mL), and large enrichment factor (26–193). The method of HFIP/ Brij-35 SUPRAS-based LPME with HPLC-DAD gave good linearity for the quantification of parabens with correlation coefficients larger than 0.9990. The limits of detection based on a signal-to-noise ratio of 3 were from 0.042 to 0.167 μg L −1 . The recoveries for the spiked real samples were in the range of 90.2–112.4% with relative standard deviation less than 8.9%. Except for tap water, one or several paraben (s) were detected in all the other real samples.
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Journal of Pharmaceutical Analysis
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2016
·
IF 0
Cao Li,Jia Xu,Dan Chen,Yuxiu Xiao
Hexafluoroisopropanol (HFIP)-induced sodium dodecyl sulfate/dodecyltrimethylammonium bromide (SDS/DTAB) catanionic surfactant coacervate extraction method coupled with high performance liquid chromatography (HPLC) was used to detect the migration of phthalates from disposable tablewares to drinking water. The concentration factors are larger than 82 and extraction recoveries over 53% for water samples spiked with 100 or 200 ng/mL phthalates. Limit of detection is in the range of 1.0–2.6 ng/mL. Good linearity with correlation coefficients larger than 0.9985 is obtained in the concentration of 20–1500 or 40–3000 ng/mL. Relative recoveries are from 82.4% to 123.6% for water samples spiked with 30/60, 250/500, and 1500/3000 ng/mL phthalates, respectively. Relative standard deviations (RSDs) are 0.4%–7.4% for intraday precision ( n =5) and 0.6%–7.8% for interday precision ( n =3). Four of studied phthalates are found in the drinking water samples prepared from four kinds of tablewares.
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ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2017
·Vol. 409
·期 19
·4559-4569
·
IF 3.431
Xu Jia,Li Yunfang,Li Cao,Zhang Rui,Xiao Yuxiu
A hexafluoroisopropanol (HFIP)-mediated cloud point extraction (CPE) system was established. A small amount of HFIP (even 1%, v / v ) can dramatically reduce the cloud point of Triton X-100 (TX-100) aqueous solution (even to 1 °C) and make liquid-liquid two-phase separation (coacervate phase and aqueous phase) occur at room temperature over a wide range of TX-100 concentration (0.5∼10%, g/mL). HFIP-mediated coacervate phase has smaller volume (volume ratio is 1.8∼8.9% relative to the volume of the total solution with 1∼5% TX-100) and larger micelle aggregates (30∼80 nm in diameter) compared to temperature-induced coacervate phase (volume ratio at 2.8∼14.0%, the diameter of micelle aggregates at 5∼30 nm). HFIP-mediated CPE was coupled to high-performance liquid chromatography with ultraviolet detection (HPLC-UV) for the extraction and detection of organic pollutants in water, namely, polycyclic aromatic hydrocarbons (PAHs), fluoroquinolones (FQs), and sulfonamides (SAs) with different polarities, charges, and hydrogen-bonding properties. HFIP-mediated CPE provides much higher extraction rates (ERs) and enrichment factors (EFs) for FQs (91∼106%, 50∼59), PAHs (63∼90%, 33∼49), and SAs (26∼55%, 16∼34) compared with the temperature-induced one (ERs: 4∼8% for FQs, 25∼46% for PAHs, and 4∼37% for SAs; EFs: 1∼3 for FQs, 6∼12 for PAHs, and 8∼13 for SAs). The limit of detection ranges from 0.24 to 0.33 ng/mL for FQs, 0.04 to 0.38 ng/mL for PAHs, and 0.63 to 1.31 ng/mL for SAs. The proposed method was applied in the analysis of real water samples, and the recovery of 79.4∼110.8% and the relative standard deviation of 0.2∼16.3% were achieved for the three types of pollutants.
Schematic illustration of HFIP-mediated cloud point extraction
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FOOD CHEMISTRY
·
2018
·
IF 4.946
Wenwen Deng,Long Yu,Xiao Li,Jia Chen,Xuanxuan Wang,Zixin Deng,Yuxiu Xiao
A series of new hydrophobic deep eutectic solvents (DESs), which are liquid at room temperature and have high density (>1.4 g mL −1 ), were synthesized using hexafluoroisopropanol (HFIP) as hydrogen-bond donor and l -carnitine/betaine as hydrogen-bond acceptor. Then these hydrophobic DESs were used as extraction solvents to establish dispersive liquid-liquid microextraction (DLLME) method for extraction of pyrethroids. The DES extraction phase was in the bottom after DLLME, being easy to be collected for analysis. After optimization by one-variable-at-a-time and response surface methodology, the enrichment factors of 265–360 were achieved for five pyrethroids. The proposed DLLME method coupled with HPLC has good performance: linear ranges of 0.25/0.5/1–100/200/400 ng/mL ( r ≥ 0.9990), limits of detection of 0.06–0.17 ng mL −1 , relative recoveries of 85.1–109.4%, intra-day and inter-day RSDs below 7.5%. The novel DLLME method is simple, rapid, highly efficient and eco-friendly for extraction of pyrethroids in real tea beverages and fruit juices.
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JOURNAL OF CHROMATOGRAPHY A
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2018
·
IF 3.716
Yu Zong,Jia Chen,Jinxuan Hou,Wenwen Deng,Xiaoyan Liao,Yuxiu Xiao
A hexafluroisopropanol (HFIP)-alkyl carboxylic acid high-density supramolecular solvent (SUPRAS) was proposed and combined with dispersive liquid-liquid microextraction (DLLME) for extraction and preconcentration of steroid sex hormones in human urine prior to analysis by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Octanoic acid was used as extraction agent and HFIP, with the properties of high density, strong hydrogen bond donor and high hydrophobicity, was used as dispersing agent of DLLME as well as coacervation-inducing agent and density-regulating agent of octanoic acid . HFIP-octanoic acid SUPRAS was spontaneously formed in the process of DLLME and located in the bottom of a urine solution due to its density higher than water. Thus, the SUPRAS phase at trace volume was easy to be collected after centrifugation using normal centrifuge tubes. Five hormones (four estrogens and progesterone) were chosen as analytes. Urine hydrolysis time, extraction conditions and derivatization conditions for estrogens were optimized. Under the optimal conditions, only 0.07 mL of organic solvent (HFIP) was consumed. An external standard calibration method was used for quantification, and a linear relationship was obtained with correlation coefficients higher than 0.9957 and p values for linear trend less than 0.0001. Limits of detection of the method based on a signal-to-noise ratio of 3 were 0.01-0.10 μg L −1 . The recoveries ranged from 82.7% to 120.2%, and intra-day and inter-day relative standard deviations of the method were less than 15%. The matrix effects of 84.0%–105.7% showed no urine matrix interferences with MS detection, which was mainly due to the restricted access property of HFIP-octanoic acid SUPRAS with reverse micelle aggregates. The absence of matrix effects contributed to the reliable quantitation by external calibration, avoiding the use of expensive isotopically labeled internal standards. The novel SUPRAS-based DLLME method, coupled with HPLC-MS/MS, was applied for determination of target hormones in real urine.
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JOURNAL OF CHROMATOGRAPHY A
·
2015
·
IF 4.169
Yu Tian,Yunfang Li,Jie Mei,Bo Cai,Jinfeng Dong,Zhiguo Shi,Yuxiu Xiao
The separation of acidic and basic proteins using CE has been limited in part due to the adsorption of proteins onto the capillary wall. In this work, the efficient control of EOF and the simultaneous separation of acidic and basic proteins are achieved by use of C 18 -4-C 18 PB as a dynamic coating additive, which is a representative surfactant for 1,1′-(butane-1,s-alkyl)bis(1-alkylpyrrolidinium) bromide (C n -4-C n PB, n = 10, 12, 14, 16 and 18). C 18 -4-C 18 PB exhibits a powerful capability in the reversal of EOF, and a low concentration even less than 0.001 mM is sufficient to reverse EOF at the tested pH values (3.0–9.0). Baseline separation of eight proteins with sharp peaks and high efficiencies (54,000–297,000 plates/m) is obtained with 30 mM NaH 2 PO 4 buffer (pH 5.0) containing 4 mM C 18 -4-C 18 PB. At the same buffer condition, the C n -4-C n PB with shorter alkyl chain ( n = 10, 12, 14, 16) cannot achieve the same effective protein separation as C 18 -4-C 18 PB. However, the combined use of small amounts (≤0.5%, v/v) of hexafluoroisopropanol (HFIP) and C n -4-C n PB ( n = 10, 12, 14, 16) as additives can completely separate all eight proteins with high efficiencies of 81,000–318,000 plates/m. The RSDs of migration time are less than 0.80% and 5.84% for run-to-run and day-to-day assays ( n = 5), respectively, and the protein recoveries are larger than 90.15%. To the best of our knowledge, this is the first report on the simultaneous separation of acidic and basic proteins using C n -4-C n PB surfactants or C n -4-C n PB surfactants combined with HFIP as dynamic coating additives.
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ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2014
·Vol. 406
·期 24
·6051-6060
·
IF 3.578
Chen Dan,Zhang Pei,Li Yunfang,Mei Zhinan,Xiao Yuxiu
Hexafluoroisopropanol (HFIP)-induced coacervation in aqueous mixed systems of catanionic surfactants of dodecyltrimethylammonium bromide (DTAB) and sodium dodecyl sulfate (SDS) was described in detail, and its application in the extraction of strongly polar sulfonamides (SAs) was investigated. With 10 % ( v / v ) HFIP inclusion, coacervation formation and two-phase separation occur in a wide range of SDS/DTAB mole ratios (88:12∼0:100 mol/mol) and total surfactant concentrations (10∼200 mmol/L). The interactions between HFIP and DTAB play an important role in coacervation formation. The HFIP-induced SDS–DTAB coacervation extraction proves to be an efficient method for the extraction and preconcentration of SAs. Both hydrophobic interaction and polar interactions (hydrogen–bond, electrostatic, and π-cation) contribute to the distribution of SAs into coacervate phase. The proposed HFIP-induced SDS–DTAB coacervation extraction combined with HPLC–UV was employed for the extraction and quantitative determination of SAs in environmental water samples. Limits of detection were 1.4∼2.5 ng mL −1 . Excellent linearity with correlation coefficients from 0.9990 to 0.9995 was obtained in the concentration of 0.01∼10 μg mL −1 . Relative recoveries were in the range of 93.4∼105.9 % for analysis of the lake, underground, and tap water samples spiked with SAs at 0.01, 1.0, and 10 μg/mL, respectively. Relative standard deviations were 0.7∼3.2 % for intraday precision and 1.3∼4.6 % for interday precision ( n = 3). Concentration factors were 17∼49 for three water samples spiked with 0.01 μg/mL SAs. The results demonstrate that the proposed extraction method is feasible for the preconcentration and determination of trace SAs in real water samples.
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ACS Sustainable Chemistry & Engineering
·
2017
·
IF 5.951
Wen-Wen Deng,Yu Zong,Yu-Xiu Xiao
Deep eutectic solvents (DESs), a new class of green and sustainable solvents, have shown a promising application prospect in the aqueous two-phase system (ATPS) extraction. In the present work, hexafluoroisopropanol (HFIP) was introduced as a hydrogen-bond donor to synthesize DESs with choline chloride (ChCl), decyltrimethylammonium bromide, dodecyltrimethylammonium bromide, and tetradecyltrimethylammonium bromide (hydrogen-bond acceptor), respectively. These HFIP-based DESs (HFIP-DESs) can form ATPS with various inorganic salts, and their phase separation ability is significantly stronger than that of small molecule aliphatic alcohols, HFIP, and traditional DESs. The ATPSs based on HFIP-DESs were first used to extract anthraquinones (AQs) from Rhei Radix et Rhizoma samples. Under the optimal conditions, more than 92% of AQs (including aloe-emodin, rhein, emodin, chrysophanol, and physcion) was enriched in the DES-rich phase of the ATPS composed of ChCl-HFIP DES and Na2SO4. Compared with the traditional chloroform extraction method (60 mL chloroform consumption), the ChCl-HFIP DES/Na2SO4 ATPS extraction method attained high extraction efficiency but only consumed 0.5 mL of organic solvent (HFIP).
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Analytical Methods
·
2026
·
IF 3
Keke Huang,Jia Chen,Wending Yao,Xiao Li
A hexafluoroisopropanol (HFIP)-induced salt-free catanionic surfactant supramolecular solvent (SUPRAS)-based direct immersion single-drop microextraction method was developed and coupled with high-performance liquid chromatography-ultraviolet detection to determine sulfonamides (SAs) and fluoroquinolones (FQs) in lake water samples. Dodecanoic acid and dodecyltrimethylammonium hydroxide were used as the salt-free catanionic surfactant pair for SUPRAS preparation, while HFIP served as the coacervate-inducing agent. Cryo-scanning electron microscopy revealed spherical micellar aggregates in the SUPRAS, which facilitated hydrophobic, hydrogen-bonding, and electrostatic interactions for analyte extraction. A novel holder, fabricated from a gel pen refill protective case, was designed to stably support the high-density SUPRAS droplet (up to 40 µL for 20 min), improving the precision and accuracy of the method. Sulfadiazine, sulfamethazine, norfloxacin, ciprofloxacin, danofloxacin, and enrofloxacin were selected as model analytes. Key factors affecting droplet stability and extraction efficiency were optimized. The method exhibited good analytical performance, with linearity (R2) > 0.9938 and limits of detection of 2.1–3.0 ng mL−1 for SAs and 0.8–1.9 ng mL−1 for FQs. Recoveries for spiked lake water samples were in the range of 81.2–106.3%, with intra- and inter-day relative standard deviations all below 7.2%. AGREEprep greenness assessment revealed that the proposed method achieved the highest score (0.45) among the compared methods, owing to its minimal organic solvent consumption, simple operation, low energy consumption, and low waste generation. Compared with reported methods, the proposed approach is simple, efficient, and environmentally benign, demonstrating strong potential for the trace determination of antibiotics in environmental water samples.
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MICROCHEMICAL JOURNAL
·
2024
·
IF 4.9
Xiao Li,Jia Chen,Caixia Yan,Xuanwei Li,Yaokun Xia,Qingwei Zhao
A novel amphiphilic supramolecular solvent (SUPRAS) was developed by hexafluoroisopropanol (HFIP)-induced self-assembly of 1,2-hexanediol in an aqueous matrix. Its application potential in multiclass determination was assessed by extracting from urine 10 prohibited hormones and metabolic modulators (log P from 2.38 to 7.57) listed by the World Anti-Doping Agency (WADA). This SUPRAS is stably formed across a wide pH range (2–12) and is unaffected by salt concentrations (<10 % g mL −1 of NaCl), and it has a higher density than water. The dehydration and hydrogen bonding ability of HFIP, as well as hydrophobic interactions between alkanediols, dominates the formation of the SUPRAS. The nanostructure of the SUPRAS, composed of 1,2-hexanediol, HFIP, and a high content of water (>25 %, w/w), forms large spherical micellar aggregates (10–100 μm) that exhibit amphiphilic properties. A 1,2-hexanediol-HFIP SUPRAS-based liquid-phase microextraction (LPME) method for detection of selected prohibited drugs in urine coupled with liquid chromatography–tandem mass spectrometry (LC-MS/MS) was established, optimized, and validated. The method showed fast extraction time (30 s of vortex) and low solvent consumption (160 μL of organic solvent). Under the optimal conditions (7 % g mL −1 of 1,2-hexanediol, 10 % v/v of HFIP), the SUPRAS achieved high extraction efficiencies (>80 %) and an enrichment factor of 6.0, with minimal matrix effects for all analytes due to its high amphiphilicity and large surface area. The method demonstrated excellent linearity (R ≥0.9909), with method limits of detection ranging from 0.018 to 0.18 ng mL −1 and method limits of quantitation ranging from 0.060 to 0.60 ng mL −1 , which are well below the minimum required performance levels set by authorities. Furthermore, the intra- and inter-day relative recoveries for spiked human urine samples varied in the ranges of 90.3–121 % and 88.1–119 %, respectively, with relative standard deviations less than 13 % and 19 %, respectively. This SUPRAS-based LPME method proves to be simple, highly efficient, and eco-friendly, and it has promising potential for multiclass determination in doping control.
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COMPOSITES SCIENCE AND TECHNOLOGY
·
2016
·
IF 3.897
Ailin Gao,Qing Yang,Lixin Xue
The crystallinity of semi-crystallized Poly ( l -Lactic acid) (PLLA) is low, especially as a porous membrane prepared from non-solvent induced phase separation (NIPS) process. To improve the crystallinity and thermal stability of PLLA porous membranes, hexafluoroisopropanol (HFIP) was added into the PLLA casting solution together with a small amount of Silk Fibroin (SF). It is found that by optimizing the additive amounts of HFIP and SF, PLLA composite membranes with improved crystallinity (up to 47.1%) and endurance to temperature (above 90 °C) could be prepared with comparable mechanical property to the virgin PLLA membranes. The effects of HFIP in NMP solution on PLLA during the NIPS process was further investigated using dynamic rheological methods relating to the crystallinity of the formed PLLA porous membranes.
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MICROCHEMICAL JOURNAL
·
2026
·
IF 5.2
Xiao Li,Xuanwei Li,Caixia Yan,Yaokun Xia,Keke Huang,Jia Chen
Alkyl carboxylic acid–HFIP SUPRAS was developed as an ideal extractant for HF-LPME. • Reversed micellar SUPRAS forms with low HFIP and is stable at low salt levels. • Hollow fiber and restricted-access SUPRAS synergistically reduce matrix effects. • Multiclass antiarrhythmic drugs in human plasma are detected by LC-MS/MS. • Low solvent/sample consumption and an AGREEprep score of 0.5 ensure eco-friendliness. An alkyl carboxylic acid–hexafluoroisopropanol (HFIP) supramolecular solvent (SUPRAS) was developed as a restricted-access solvent for hollow fiber liquid-phase microextraction (HF-LPME) and applied to the determination of seven antiarrhythmic drugs (mexiletine, propranolol, diltiazem, amlodipine, propafenone, verapamil, and amiodarone) in human plasma. SUPRAS formation required only a low HFIP dosage (<10%, v /v for alkyl carboxylic acid ≤4%, w / v ) and was minimally affected by low ionic strength (NaCl <50 mM) or low organic solvent content (methanol <5%, v /v). The SUPRAS consisted of reversed micellar aggregates with hydrophobic outer surfaces and hydrophilic inner cavities. The SUPRAS exhibited restricted-access behavior, efficiently excluding macromolecular proteins (extraction efficiency <18.3%, solubility <4.5 mg mL −1 ) via the synergistic effects of protein denaturation/flocculation induced by HFIP and octanoic acid and size exclusion by the SUPRAS matrix. After systematic optimization, the proposed method coupled with high-performance liquid chromatography-tandem mass spectrometry demonstrated acceptable analytical performance. Satisfactory linearity was achieved, with correlation coefficients ranging from 0.9903 to 0.9997. Method limits of detection (S/N = 3) ranged from 0.01 to 0.10 μg L −1 , while method limits of quantification (S/ N = 10) were 0.03–0.33 μg L −1 . Acceptable recoveries were obtained for spiked samples (86.5–126.6%), with only two analytes slightly exceeding 130% at the low concentration level, and intra- and inter-day precisions were below 19.3%. Owing to the combined microfiltration capability of the hollow fiber and the restricted-access properties of the SUPRAS, the method exhibited manageable matrix effects (70.6–132.5%) and eliminated the need for a separate protein precipitation step, while consuming only 25 μL of SUPRAS per extraction. Greenness assessment using AGREEprep software yielded a score of 0.5, confirming satisfactory eco-friendliness and sustainability. This SUPRAS-HF-LPME method is simple, efficient, and environmentally benign, serving as a promising pretreatment and quantification strategy for antiarrhythmic drugs in complex human plasma matrices. Download: Download high-res image (265KB) Download: Download full-size image
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