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1.
Analyst ; 2024 Aug 30.
Article in English | MEDLINE | ID: mdl-39212070

ABSTRACT

The recombinant Cluster of Differentiation 40 Ligand (CD40L) can be expressed in various cells and is closely related to various types of cancer. This association underscores the critical need for expedited and precise measurement of CD40L levels in clinical fluid specimens. A novel optical fiber biosensor has been devised, employing single-mode fibers that are sandwiched around a coreless fiber, with the diameter refined by etching with hydrogen fluoride. This innovative configuration allows for light transmission through the evanescent field, thereby enhancing the sensor's sensitivity to changes in the surrounding refractive index. Employing chemical binding techniques, CD40 was securely immobilized onto the fiber's surface, facilitating the detection of CD40L. The sensor exhibited a sensitivity of 1.126 nm (µg mL-1)-1 and a detection limit of 0.68 nM. Furthermore, the sensor's specificity for CD40L was validated using authentic clinical serum samples spiked with artificial analytes. In addition, the specificity of CD40L of the proposed sensor was proved using natural clinical serum samples with added artificial analyte, assisted by the ELISA method, and the results ideally conformed with the detection of standard samples. With the aid of the ELISA method, the outcomes were found to be in excellent agreement with those from standard sample detection. Consequently, the findings indicate that this sensor provides a specific, label-free, and highly sensitive method for CD40L detection, showcasing its significant potential for applications in molecular biology research.

2.
Talanta ; 271: 125673, 2024 May 01.
Article in English | MEDLINE | ID: mdl-38244311

ABSTRACT

Photoionization-ion trap mass spectrometry (PI-ITMS) is one of the major directions of mass spectrometer miniaturization because of its great potential for rapid on-site VOCs detection in many cases. Traditionally, PI has always been investigated separately and is restrained by ion transmission structure, so a new structure needs to be designed and investigated for simplifying and improving the ion transmission efficiency. Interestingly, our preliminary experiments found that the signal intensity and mass range can be effectively improved by combing atmospheric pressure photoionization (APPI) and low-pressure photoionization (LPPI). Therefore, in this paper, a new dual photoionization - ion trap mass spectrometry (DPI-ITMS) was developed, explored and used to directly analyze complex VOCs. Compared with traditional single PI configuration, it presents two obvious merits: (1) simplified ion transmission structure, eliminating the need to use deflection electrode to repel ions and avoiding breakdown risk. (2) some missing/weak low m/z ion mass spectral peaks in APPI and some high m/z ion mass spectral peaks in LPPI were improved in DPI detection mode. In addition, by combining multivariate statistical analysis, we preliminary achieved in differentiating fruit types and maturity level. In summary, we concluded that the developed DPI-ITMS has moderate detection sensitivity (limited by the homemade ITMS, 0.1-1 ppmv with RSD of 6.36 %), and the DPI-ITMS configuration can be referenced by future PI-MS, and this study also provides a high-throughput, simple, noninvasive and no chemical contamination solution for analyzing main VOCs in fruit aroma.


Subject(s)
Fruit , Odorants , Gas Chromatography-Mass Spectrometry , Atmospheric Pressure , Drug Contamination
3.
Rapid Commun Mass Spectrom ; 37(24): e9648, 2023 Dec 30.
Article in English | MEDLINE | ID: mdl-37953544

ABSTRACT

RATIONALE: By applying radio frequency (RF) and direct current (DC) voltages to corresponding ring electrodes, ion funnel (IF) can efficiently focus and transmit ions. However, IF has an inherent mass discrimination problem that will greatly limit low mass-to-charge (m/z) ion focusing and transmission. To improve the transmission efficiency (TE) of the IF, this paper explores three new profile quadrupole ion funnels (QIF). METHODS: Computer simulations of the potential field distributions of QIFs and conventional IFs were performed to assess their focusing characteristics. To compare the TE, ion optics simulation programs SIMION and AXSIM were used to perform a series of simulations. Three QIF types (toroidal, cylindrical, and hyperbolic configurations) were used to improve ion TE, and their transmission and focus performance were also compared with conventional IF. RESULTS: By simulating the trajectories of ions in the IF, the optimum electrical parameters for three new QIFs were obtained and compared with conventional IFs, with TE improvements recorded for m/z < 100 of 16%, 20%, and 13%. CONCLUSIONS: The results indicate that studying these three new IF configurations has great research significance for improving sensitivity to low m/z ions in mass spectrometer instruments.

4.
Org Lett ; 25(46): 8302-8307, 2023 Nov 24.
Article in English | MEDLINE | ID: mdl-37966133

ABSTRACT

An efficient asymmetric [1,3] O-to-C rearrangement of quinolin-2(1H)-ones enabled by a chiral bisoxazoline/copper complex has been developed. This strategy tolerated a wide range of substrates to provide a series of 1,4-dihydroquinoline-2,3-diones containing a quaternary stereocenter. A further cyclization of the [1,3] O-to-C rearrangement products was also realized, which led to various optically active 3,4-dihydroquinolin-2-ones with broad substrate scope.

5.
J Am Soc Mass Spectrom ; 34(8): 1805-1812, 2023 Aug 02.
Article in English | MEDLINE | ID: mdl-37463266

ABSTRACT

The SPIN tandem ion funnel (IF) structure allows for highly sensitive mass spectrometry due to reduced ion losses in the interface region and during transmission; however, IF has an inherent mass discrimination problem, which can greatly restrain the ion transmission efficiency (TE) and therefore requires certain optimization methods. Conventional optimization methods ignore the combined effects of multiple IF characteristic parameters (electrical and dimensional parameters) and are unable to achieve efficient ion transmission over a wide mass range, thus requiring significant tuning time. In this paper, a genetic algorithm (GA)-optimized printed circuit board ion funnel (PCBIF) was designed, fabricated, preliminarily evaluated, and integrated into the SPIN interface to address the ion loss that can occur when mass spectrometers transfer ions at subambient pressure. Simulation studies have showed clearly that the effective automated GA can increase the PCBIF optimization, design, and the ion TE (finding the optimal characteristic parameters within 4 h and achieving 96% ion TE for ions with m/z between 50 and 700). Preliminary tests on built SPIN-PCBIF-MS can lead to an LOD of 0.01 nM and also indirectly suggest the effectiveness of the GA-optimized PCBIF. The proposed GA method helps to guide the design of IF and can also be used for other multivariate mass analyzers or ion transmission devices.

6.
Talanta ; 253: 123995, 2023 Feb 01.
Article in English | MEDLINE | ID: mdl-36228553

ABSTRACT

Mass spectrometry is an indispensable technology for the characterization of glycans. However, specific identification of isomeric glycans especially sialylated glycan isomers using mass spectrometry alone is challenging, which is why orthogonal techniques are needed. Aiming to achieve simple, rapid, and specific identification of sialyl-linkage isomers, we reported herein a trapped ion mobility spectrometry time of flight mass spectrometry (TIMS-TOF MS) method for linkage-specific identification of sialylated glycans through conjugation with metal complexes. Two pairs of sialyl-linkage isomers including 3'/6'-sialyllactose (3'/6'-SL) and 3'/6'-sialyl-N-acetyllactosamine (3'/6'-SLN) conjugated with the diethylenetriamine (DETA) or 2,2'; 6',2″-terpyridine (Terpy) ligand and transition metal ion (Mn2+, Fe2+, Co2+, Ni2+, Cu2+, or Zn2+) were studied by TIMS-TOF MS. The two pairs of sialylated isomers were successfully separated with a metal-ligand system, and relative quantification of sialyl-linkage isomers was demonstrated. In addition, the linkage of the sialic acid moiety can also be distinguished with MS/MS in combination with the metal-ligand system.


Subject(s)
Coordination Complexes , Ligands , Tandem Mass Spectrometry
7.
Anal Chem ; 94(51): 17827-17834, 2022 12 27.
Article in English | MEDLINE | ID: mdl-36512629

ABSTRACT

Development of fragment ion detection methods is of great importance for mass spectrometer advancement or substance identification. To date, collision induced dissociation (CID) remains the most commonly used ion activation method in MS/MS experiments, and the effectiveness of CID in an ion trap mass spectrometer is limited by low mass cutoff and weak fragmentation yields. Theoretically, controlling the q value is the key to maintain the fragment efficiency and trapping efficiency of MS/MS, thus improving the detection of fragment ion, while currently reported techniques usually require complex circuitry and often produce different CID patterns. In this paper, with the developed synchronized reversed scanning-collision induced dissociation (SRS-CID) technique, we demonstrate its effective improvement in fragment ion detection. The SRS-CID is implemented on a digital ion trap mass spectrometer (DITMS) by reverse scanning the q values during CID process, or specifically, the frequency is increased during the CID process. With the SRS-CID technique, the fragmentation efficiency of precursor ions can be slightly improved. For reserpine analyte, the trapping efficiency for low-mass fragment ions is improved at least 3 times, and for YGGFL, the trapping efficiency for low-mass fragment ions is improved at least 9 times. These experimental results can also be validated by simulations, and the kinetic energy variation plot suggests consecutive fragmentation occurs. In any case, the SRS-CID provides a solution to the low efficiency of fragment ion detection during tandem MS analysis, which will certainly be useful in the future.


Subject(s)
Tandem Mass Spectrometry , Tandem Mass Spectrometry/methods , Ions
8.
Pain Physician ; 25(8): E1279-E1287, 2022 11.
Article in English | MEDLINE | ID: mdl-36375201

ABSTRACT

BACKGROUND: Percutaneous balloon compression (PBC) is a safe and effective method to treat trigeminal neuralgia. Despite it is known that intraoperative balloon volume is crucial in the prognosis of PBC patients and correlates with Meckel's cave (MC) size, it is a lack of objective and valid criteria for intraoperative balloon volume of PBC. OBJECTIVES: The aim of this study was to evaluate the relationship between the size of MC and the volume of a pear-shaped balloon in improving the prognosis of patients receiving PBC. STUDY DESIGN: Retrospective study. METHODS: Patients were divided into 3 groups according to their prognosis, and simple linear regression equations were established separately. Group A was defined as having recurrence. Group B was defined as having no recurrence and a Barrow Neurological Institute facial numbness (BNI-N) score of 2 with no recurrence. Correlation analysis was carried out to determine the association of the intraoperative balloon volume with MC size. We attempted to construct simple linear regression models after verifying that both parameters were in compliance with the requirements of this model. RESULTS: Until the end of the 6-months follow-up, 60 patients (93.8%) reported no pain, and 4 patients (6.3%) experienced no significant pain relief. Sixteen (25.0%) patients had severe facial numbness, 48 (75.0%) patients had no facial numbness or had only mild numbness. All 3 groups had a significant correlation between balloon volume and MC size. Group A: Balloon volume (cm3) = -0.371 + 1.883*MC size (R2 = 0.882); Group B: Balloon volume (cm3) = 0.110 + 1.274*MC size (R2 = 0.861); and Group C: Balloon volume (cm3) = 0.011 + 1.835*MC size (R2 = 0.857). LIMITATIONS: The main limitation of our study is its observational retrospective nature, and we were unable to further analyze the intraoperative balloon pressure and volume, as well as validate the accuracy of the model. In additional this was a single-center study with a small sample size and a short follow-up period. These may have contributed to the bias in the final results. A multicenter, prospective study with a large sample size should be performed to further investigate the long-term effects of individualized balloon volumes and the correlation between pressures. CONCLUSIONS: The equation [balloon volume (cm3) = 0.110 cm3 + 1.274*MC size] yields an appropriate value at which the patient has a low recurrence rate and a low degree of facial numbness. Preoperative measurement of MC size can be used to guide the intraoperative balloon volume and to predict the patient's prognosis.


Subject(s)
Trigeminal Neuralgia , Humans , Trigeminal Neuralgia/surgery , Retrospective Studies , Hypesthesia , Prospective Studies , Prognosis , Magnetic Resonance Imaging/methods , Treatment Outcome
9.
Analyst ; 147(24): 5764-5774, 2022 Dec 05.
Article in English | MEDLINE | ID: mdl-36413223

ABSTRACT

The study and design of high-resolution mass analyzers is a very important task in mass spectrometry. A planar electrostatic ion trap (PEIT) mass analyzer with image charge detection and FT-based data processing has been developed, theoretically simulated, and experimentally validated. However, the 10 ring electrode configuration (PEIT-10) is difficult for mechanical construction and voltage tuning; moreover, few methods have been reported for optimizing the performance of multi-electrode mass analyzers. In this article, a simplified PEIT-7 mass analyzer was designed, and a genetic algorithm parallel optimization (GAPO) method was developed for optimizing multiple voltage settings of the new PEIT-7 mass analyzer to achieve spatial and energy isochronicity as well as iso-coordinate property. The automatic voltage optimization processes for the reduction of time aberration and spatial aberration showed that the developed GAPO method can significantly improve the optimization efficiency (the optimal voltage set being found within 5 hours with a maximum time aberration of 15 ps and a maximum z aberration of 0.10 µm). Based on the results obtained from the GAPO method, the resolving power of the PEIT-7 mass analyzer for six groups of ions with closely packed masses (m/z = 117.000 Th to 117.010 Th) was demonstrated, and a mass resolution of 171k was achieved at an acquisition time of 200 ms. The established GAPO method facilitates the design and optimization of high-resolution mass analyzers and may be useful for the design of other multi-electrode ion optical devices.

10.
Anal Bioanal Chem ; 414(27): 7885-7895, 2022 Nov.
Article in English | MEDLINE | ID: mdl-36136112

ABSTRACT

In this work, on the basis of an immobilized metal ion affinity chromatography enrichment strategy, a new kind of covalent organic framework (COF) material for enrichment of phosphorylated peptides and exosomes was successfully prepared in a facile method, and Ti4+ and Nb5+ were used as dual-functional ions (denoted as COF-S-S-COOH-Ti4+/Nb5+). With the advantage of unbiased enrichment towards phosphopeptides, COF-S-S-COOH-Ti4+/Nb5+ shows ultra-high selectivity (maximum molar ratio of ß-casein: BSA is 1:20,000) and low limit of detection (0.2 fmol). In addition, the material has an excellent phosphopeptide loading capacity (100 µg/mg) and reusability (at least seven times). Furthermore, applying the material to the actual sample, 4 phosphopeptides were selectively extracted from the serum of renal carcinoma patients. At the same time, exosomes with an intact structure in the serum of renal carcinoma patients were successfully isolated rapidly using this strategy. All experiments have shown that COF-S-S-COOH-Ti4+/Nb5+ exhibits exciting potential in practical applications.


Subject(s)
Carcinoma, Renal Cell , Exosomes , Kidney Neoplasms , Metal-Organic Frameworks , Caseins/chemistry , Chromatography, Affinity/methods , Exosomes/chemistry , Humans , Imidazoles , Ions , Niobium/chemistry , Phosphopeptides/analysis , Titanium/chemistry
11.
Clin J Pain ; 38(11): 686-692, 2022 11 01.
Article in English | MEDLINE | ID: mdl-36173138

ABSTRACT

OBJECTIVE: This study aimed to investigate the effect of therapy with peripheral nerve stimulation (PNS) and pulsed radiofrequency (PRF) combined or PNS and PRF separately in patients with herpes zoster ophthalmicus (HZO). MATERIALS AND METHODS: This cohort study included 106 cases of HZO. Three groups were identified according to the type of treatment received: combination therapy (PNS+PRF) (n=38), PRF (n=37), and PNS (n=31). The observations at 0, 1, 2, and 4 weeks; 3 and 6 months; and 1 and 2 years after the operation were analyzed. Observations at each follow-up included baseline characteristics, Numerical Rating Scale (NRS) and the Pittsburgh Sleep Quality Index (PSQI), concomitant pain medication usage, relapse rate, and adverse events. RESULTS: The postoperative NRS of all 3 groups were significantly lower than preoperative scores. The PSQI of the 3 groups was significantly improved postoperatively, and the concomitant pain medication gradually decreased. Regarding long-term efficacy, the pain NRS and PSQI scores of the PNS+PRF and PNS groups were significantly lower than those of the PRF group ( P <0.05), and the relapse rate of the PRF group was higher than that of the PNS+PRF and PNS groups ( P <0.05). No significant difference was observed between the PNS+PRF and the PNS groups. CONCLUSION: Both PNS and PRF treatment of HZO can decrease the pain score, yielding no serious complications. The combination of PNS and PRF or PNS alone resulted in more significant pain relief than treatment with PRF alone. Thus, PNS therapy may be a better treatment option for HZO.


Subject(s)
Herpes Zoster Ophthalmicus , Herpes Zoster , Neuralgia , Pulsed Radiofrequency Treatment , Cohort Studies , Herpes Zoster/complications , Herpes Zoster Ophthalmicus/complications , Herpes Zoster Ophthalmicus/therapy , Humans , Neuralgia/complications , Neuralgia/therapy , Peripheral Nerves , Pulsed Radiofrequency Treatment/methods , Recurrence , Treatment Outcome
12.
Front Mol Neurosci ; 15: 938280, 2022.
Article in English | MEDLINE | ID: mdl-36034501

ABSTRACT

Introduction: The efficacy of short-term spinal cord stimulation (stSCS) as a treatment for neuropathic pain in patients with postherpetic neuralgia (PHN) has already been validated. However, the potential alterations in brain functionality that are induced by such treatment have yet to be completely elucidated. Methods: This study use resting-state functional magnetic resonance imaging (rs-fMRI) to detect the changes in regional homogeneity (ReHo) and degree centrality (DC) related to stimulator-induced pain relief in patients with PHN. A total of 10 patients with PHN underwent an MRI protocol at baseline and after stSCS. Alterations in ReHo and DC were then compared between baseline and after stSCS. We investigated the relationship between clinical parameters and functional changes in the brain. Results: Clinical parameters on pain, emotion, and sleep quality were correlated with ReHo and DC. ReHo and DC were significantly altered in the middle temporal gyrus, precuneus, superior frontal gyrus, supramarginal gyrus, inferior parietal lobule, rolandic operculum, middle occipital gyrus, superior parietal gyrus, and the precentral gyrus after stSCS. A significant correlation was detected between ReHo changes in the middle occipital gyrus, precuneus, inferior parietal gyrus, and changes in pain, emotion, and sleep quality. A significant negative correlation was detected between DC changes in the middle temporal gyrus, rolandic operculum, supramarginal gyrus, precuneus, inferior parietal gyrus, and changes in pain, emotion, and sleep quality. Conclusion: This study found that stSCS is able to induce ReHo and DC changes in patients with PHN, thus suggesting that stSCS can change brain function to alleviate pain, sleep, and emotional disorder.

13.
J Am Soc Mass Spectrom ; 33(6): 898-906, 2022 Jun 01.
Article in English | MEDLINE | ID: mdl-35475621

ABSTRACT

Nonvolatile compounds usually have a high molecular weight and exhibit a high boiling point, which poses great challenges to the ionization method of MS. Ambient ionization sources can efficiently analyze the nonvolatile compounds without complex pretreatment, but they generally require special media such as heating devices, laser optical devices, or corona needles. Acoustic nebulization assisted photoionization (ANPI) is a potential method for the analysis of nonvolatile compounds that uses nebulization as a prerequisite for photoionization and introduces many advantages of PI, including excellent ionization efficiency, a high yield of molecular ions, and simplified spectrum interpretation. However, the ANPI source can be limited in on-site applications by the complexity of the analytical devices and the high cost of the nebulization chip. To address this issue, in this paper, we explored cheap and commercially piezoelectric materials used in a mist sprayer and fabricated a nebulization swab assisted photoionization (NSAP) as an ambient ionization source. Some useful results are presented: numerical simulation was introduced successfully for optimizing the aerosol distribution in the NSAP source; nonvolatile muscle relaxants, drugs of abuse, antibiotics, phthalates, and cholesterol were detected mostly as their protonated molecular ions while some special acetone/water cluster ions were detected. In addition, the LOD for most of the target analytes ranged from 10.0 to 50.0 pg with RSD ≤ 9%. Finally, this method is implemented for Chinese baijiu spiked with phthalates. The experimental data shows the capability of a NSAP source in high sensitivity and on-site analysis of the nonvolatile compounds.


Subject(s)
Acetone , Acoustics , Gas Chromatography-Mass Spectrometry , Ions , Mass Spectrometry/methods
14.
Talanta ; 243: 123363, 2022 Jun 01.
Article in English | MEDLINE | ID: mdl-35272154

ABSTRACT

Chiral recognition is of highly interest in the areas of chemistry, pharmaceuticals, and bioscience. An effective strategy of enantiomeric determination of amino acids (AAs) was developed in this work. All 19 natural AAs enantiomers can be easily distinguished by ion mobility-mass spectrometry of the non-covalent complexes of AAs with cyclodextrins (α-CD, ß-CD and γ-CD) and Mg2+ without any chemical derivatization. Differences of the mobilities between the enantiomers' complexes is from 0.006 to 0.058 V s/cm2. In addition, the complex of [ß-CD + Phe + Mg]2+ was selected as an example to study the relative quantification by measuring L/D-Phe at different molar ratio of 10:1 to 1:10 in the µM range, resulting in a good linearity (R2 > 0.99) and high sensitivity at 2 µM. A DFT calculation was also performed to illustrate the detailed molecular structure of the complexes of CDs, Mg2+ and D- or L-Phe. Both experiment and theoretical calculation showed that Mg2+ plays an important role in host/guest interactions, which changed the molecular conformations by non-covalent interaction between Mg2+ and CDs, and resulted in the different collision cross-sections of the complex ions of CDs, Mg2+ and D- or L-AAs in the gas phase. This effective and convenient strategy could potentially be utilized in scientific research and industry for routine enantiomeric determination of natural AAs, peptides and some other small chiral biomolecules such as non-natural AAs and carboxylic acid-containing drugs.


Subject(s)
Cyclodextrins , Ion Mobility Spectrometry , Amino Acids/analysis , Cyclodextrins/chemistry , Density Functional Theory , Ions , Stereoisomerism
15.
Anal Chem ; 94(8): 3553-3564, 2022 03 01.
Article in English | MEDLINE | ID: mdl-35179030

ABSTRACT

Discrimination of isomers is an important and valuable feature in many analytical applications, and the identification of chiral isomers and cis-trans isomers is the current research focus. In this work, a simple method for direct, simultaneous recognition of d-/l-proline (P), d-/l-/cis-/trans-4-hydroxyproline (4-HP), and d-/l-/cis-/trans-N-tert-butoxycarbony (N-Boc-4-HP) was investigated by means of trapped ion mobility spectrometry-mass spectrometry (TIMS-MS). The isomers with cis-/trans-/d-/l-configuration can be directly recognized based on their mobility upon reaction with natamycin (Nat) and metal ions through noncovalent interactions. The results indicate that the recognition of the enantiomers has certain specificity, and the structural difference of the enantiomers was increased in a complex with Nat and metal ions. Herein, d-/l-P can be recognized through the ternary complexes [P + Nat + Mg - H]+, [P + 2Nat + Ca - H]+, [P + 2Nat + Mn - H]+, and [P + Nat + Cu - H]+. Similarly, c-4-HPL, c-4-HPD, t-4-HPL, and t-4-HPD can be recognized by [4-HP + Nat + Ca - H]+, [4-HP + 2Nat + Ca - H]+, and [4-HP + Nat + Cu - H]+, while N-Boc-c-4-HPL, N-Boc-c-4-HPD, N-Boc-t-4-HPL, and N-Boc-t-4-HPD were recognized through the enantiomer complexes [N-Boc-4-HP + Nat + Li]+, [N-Boc-4-HP + Nat + 2Na - H]+, [N-Boc-4-HP + Nat + K]+, [N-Boc-4-HP + Nat + Mn - H]+, and [N-Boc-4-HP + Nat + Ba - H]+. Moreover, tandem mass spectrometry (MS/MS) results indicated that different collision energies were obtained for the same fragment ions, which implied that the enantiomer complexes that contributed to their mobility separation shared identical interaction mode but had different gas-phase rigid geometries. Furthermore, the relative quantification for the enantiomers was performed, and the results were supported by a satisfactory coefficient (R2 > 0.99). The developed method can provide a promising and powerful strategy for the separation of chiral proline and its d-/l-/cis-/trans derivatives, bearing the advantages of higher speed, better accuracy, high selectivity, and no need for chemical derivatization and chromatographic separation.


Subject(s)
Proline , Tandem Mass Spectrometry , Ion Mobility Spectrometry , Ions , Natamycin , Stereoisomerism , Tandem Mass Spectrometry/methods
16.
Anal Bioanal Chem ; 414(4): 1493-1501, 2022 Feb.
Article in English | MEDLINE | ID: mdl-34505165

ABSTRACT

In this study, a special poly solid-phase extraction (in-tube SPE) column consisting of poly (POSS-octavinyl-co-N-methylacetamide-co-divinylbenzene) [poly (POSS-OS-co-DVB-co-NMA)] was prepared based on the chemical structure of the preservatives, and was used as medium for extraction analysis in combination with UPLC. The composition of polymer SPE was optimized and characterized; good scanning electron microscopy (SEM) properties and satisfactory porosity were obtained with 30% monomer (POSS-OS:DVB:NMA = 2 wt%:13 wt%:15 wt%) and 70 wt% porogenic solvent (PEG20000:DMSO:ACN = 10 wt%:50 wt%:10 wt%). The experimental parameters of the in-tube SPE-UPLC analysis were optimized systematically. Then, the in-tube SPE-UPLC method was applied for analyzing the beverage sample, and correlation coefficients (R2) > 0.99 were obtained for the linear relationship within limits of 0.1~5.0 µg mL-1. Excellent extraction efficiency, good precision, and satisfactory limit of detection sensitivity between 0.03 and 0.10 µg mL-1 were obtained. The recovery ranged from 71.5 to 88.0%, with RSD ≤ 6.1%. Furthermore, the proposed method has the features of simple sample pretreatment, high throughput, rapid analysis, cost-effectiveness, and satisfactory sensitivity. Hence, the developed in-tube SPE-UPLC method based on the poly (POSS-OS-co-DVB-co-NMA) SPE column can be potentially used for simple and sensitive detection of preservatives.

17.
Anal Chem ; 93(45): 15096-15104, 2021 11 16.
Article in English | MEDLINE | ID: mdl-34726389

ABSTRACT

The separation of chiral enantiomers has gained increasing importance in many research fields, becoming a major research hotspot. 1,1'-Bi (2-naphthol) (BINOL) and 1,1'-binaphthyl-2,2'-diyl hydrogen phosphate (BNP) are referred to as atropisomer chiral molecules, which are essential chiral catalysts and intermediates in several reactions. In this work, BINOL and BNP atropisomers are separated and identified using trapped ion mobility spectrometry (TIMS) to monitor the different mobilities of their derivative complexes. The latter are obtained by the simple mixing of BINOL/BNP, cyclodextrin (CD), and the metal ions through noncovalent interactions. The results indicate that the enantiomer complexes of BINOL/BNP can be separated with a certain specificity, showing that R-, S-BINOL can be separated by the ternary complexes of [BINOL+γ-CD + Rb]+, [BINOL+γ-CD + Cu-H]+, and [BINOL+ß-CD + Cu-H]+ based on the difference in their mobility; similarly, the R-, S-BNP enantiomer can be isolated by the formed ternary complexes of [BNP+α-CD + Ba-H]+, [BNP+ß-CD + Co-H]+, [BNP+ß-CD + Ca-H]+, [BNP+ß-CD + Cu-H]+, [BNP+ß-CD + Fe-H]+, [BNP+ß-CD + Li]+, and [BNP+ß-CD + Sr-H]+. Furthermore, the peak separation rate (Rp-p) of the complexes was calculated, with the Rp-p of the three enantiomers of BINOL being 1.130 and the Rp-p of the seven complexes of BNP reaching 2.089. At last, the different survival yields for the collision energies were found for the enantiomer complexes, revealing the rigid structural differences in the stereospecificity of the enantiomer complexes that result in the separation by the TIMS. Additionally, due to the advantages of simple operation, fast speed, and high sensitivity and because chemical derivatization and chromatographic separation are not required, the developed method can provide a promising and powerful strategy for the separation and identification of binaphthyl derivatives or even other enantiomers of the reaction intermediates.


Subject(s)
Cyclodextrins , Ion Mobility Spectrometry , Ions , Naphthols , Phosphates , Stereoisomerism
18.
Pain Physician ; 24(8): E1255-E1262, 2021 12.
Article in English | MEDLINE | ID: mdl-34793652

ABSTRACT

BACKGROUND: Recurrent trigeminal neuralgia (TN) after surgical operations can be quite difficult to treat, and treatment measures have not been standardized. Patients often have long-term, repeated severe pain, which may easily cause anxiety and depression and can exert a negative effect on the quality of life. Despite the known efficacy of percutaneous balloon compression (PBC) for TN, it is unclear whether PBC can be used as the preferred surgical treatment for postoperative recurrent TN and effectively improve patients' negative emotions. OBJECTIVES: This study aimed to evaluate the clinical curative effect of PBC in patients with postoperative recurrent TN and analyze the improvement in conditions such as anxiety, depression, and sleep disorders. STUDY DESIGN: Retrospective study. SETTING: Center of Pain Medicine, Department of Anesthesiology, pain, and Perioperative Medicine, the First Affiliated Hospital of Zhengzhou University. METHODS: Clinical data from 121 postoperative recurrent TN patients who underwent PBC between August 2017 and June 2019 were retrospectively reviewed and analyzed. The Barrow Neurological Institute pain intensity (BNI-P) score was used to measure the severity of pain. The Hospital Anxiety and Depression Scale (HADS) and Pittsburgh Sleep Quality Index (PSQI) were used to evaluate anxiety, depression, and sleep status. RESULTS: On postoperative day 1, 104 patients (86.0%) reported no pain, 9 patients (7.4%) had occasional pain that did not require medication, and 8 patients (6.6%) experienced no significant pain relief. The total efficacy was 93.4%. Moreover, 3 patients (2.5%) reported significant pain relief 2 weeks postoperatively. Within a follow-up time of 12 months, 101 (83.5%) patients remained pain-free, while 5 patients (4.1%) experienced recurrence. Taking into account economic factors, the patients were tolerant to pain after taking medication and did not undergo repeated PBC. Forty-six patients (38.0%) suffered from anxiety, 70 patients (57.9%) had depression, and 62 patients (51.2%) had poor sleep quality preoperatively. There were significant improvements in anxiety, depression, and sleep status postoperatively compared with preoperatively. Postoperative side effects included facial numbness in 115 patients (95.0%), masticatory muscle weakness in 86 patients (71.1%), herpes simplex in 18 patients (14.9%), and diplopia secondary to abducens nerve palsy in 2 patients (1.7%). None of the patients had corneal anesthesia, anesthesia dolorosa, aseptic meningitis, cerebrospinal fluid leakage, subarachnoid hemorrhage, carotid cavernous fistula, or death in this study. LIMITATIONS: This study was a single-center retrospective study, the sample size was small, and the follow-up time was relatively short. Therefore, the long-term efficacy of PBC for postoperative recurrent TN needs further evaluation from multiple centers with a large sample size and long-term follow-up. CONCLUSIONS: PBC is a minimally invasive, safe, and effective procedure. Moreover, it significantly improves the symptoms of anxiety, depression, and sleep quality caused by TN, so it appears to be regarded as an optimized choice for patients with recurrent TN after surgical procedures.


Subject(s)
Radiosurgery , Trigeminal Neuralgia , Emotions , Humans , Quality of Life , Retrospective Studies , Sleep Quality , Treatment Outcome , Trigeminal Neuralgia/surgery
19.
Analyst ; 146(21): 6455-6462, 2021 Oct 25.
Article in English | MEDLINE | ID: mdl-34596639

ABSTRACT

Linear ion trap mass analyzer could improve analytical performance compared to the traditional three-dimensional ion trap. In this study, a systematic investigation of the effect of octopole field on the performance of linear quadrupole ion trap was studied by both theoretical simulations and experiments. An asymmetric semi-circular linear ion trap (AsC-LIT) analyzer was designed and tested based on the theoretical results. The AsC-LIT consists of one pair of larger semi-circular rods with radius Ry and one pair of smaller semi-circular rods with radius Rx (Ry > Rx) in the cross section for introducing the quantitative octopole field. The analytical performances of these simplified AsC-LITs with different amounts of octopole fields were carefully investigated using both theoretical simulations and experimental validation. Experimental results showed that it could have a mass resolution of 1645 at m/z 175 (arginine); furthermore, the low mass cutoff and CID efficiency can be significantly improved when some positive octopole is added. The simulative results indicated that 2.56% octopole component was the best choice for achieving higher analytical performances. The theoretical and experimental studies of this work could certainly enrich the knowledge of a higher order electric field effect on the linear ion trap, furthermore, the simple geometric design and performance characteristics of this new AsC-LIT make it particularly attractive in the development of miniaturized mass spectrometers.

20.
Analyst ; 146(12): 3810-3817, 2021 Jun 14.
Article in English | MEDLINE | ID: mdl-33977965

ABSTRACT

The effective electric field radius is a fundamental parameter of ion traps, and it has a significant influence on ion-trapping capability, signal intensity, mass range and some other properties of the ion trap. For a quadrupole ion trap built with ideal hyperbolic electrodes, its effective electric field radius can be obtained by its geometrical size, while it is very difficult to obtain the effective electric field radius for a non-hyperbolic ion trap. In this study, the effective electric field radius of a linear ion trap and some ceramic rectilinear ion traps (cRITs) were investigated via the digital ion trap technology. The dipole frequency of supplementary AC for excitation was locked at a certain value of the main RF trapping wave, and the characteristic q values for excitation could be determined accordingly. The q values could be further used to calculate the effective electric field radius through theoretical calculations. A linear equation had been fitted between the q values for excitation and the square of period T2 through experiments subsequently. The relative deviation between the measured electric field radius and the simulative electric field radius is less than 2%. The simulation results and experimental validation show that the approach has predictive power for modeling and measuring the effective field radius of non-hyperbolic ion traps. It is certainly significant for further understanding the performances of non-hyperbolic quadrupole systems.

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