ABSTRACT
BACKGROUND: Eltrombopag Olamine is a drug used to treat thrombocytopenia, a disorder where blood platelet counts get lower and severe aplastic anemia. It serves as a thrombopoietin receptor agonist, which give rise to platelet production in the bone marrow. OBJECTIVES: The objective of this study is to develop a simple, specific, accurate, precise and economical Ultraviolet spectroscopy method to estimate the amount of Eltrombopag Olamine in bulk and tablet dosage form. METHODS: The developed method was performed using methanol for identification and physicochemical characterization of the drug. The validation parameters like linearity, precision, accuracy, robustness limits of detection and quantitation, and specificity were assessed as per ICH Q2 (R2). RESULTS: The maximum absorbance wavelength (λmax) of the drug was found at 247 nm in methanol. The linearity was found in the concentration range of 2-14 µg/ml with regression equation y = 0.0619x - 0.0123 and r² = 0.999. The standard addition method was used to determine the accuracy of the developed method. The result was found in the % recovery range of 98-99%. The precision was done on λmax with respect to the parameters such as repeatability, intraday, and interday. The method was found to be precise as the % RSD value was found to be <2%. The detection limit value (LOD) and quantitation limit value (LOQ) were 0.0524 µg/ml and 0.1588 µg/ml, respectively. CONCLUSION: The developed method is simple, economical, accurate and selective. The developed method was adaptable for the estimation of Eltrombopag Olamine analysis in pharmaceutical dosage form and routine quality control laboratory.
Subject(s)
Benzoates , Hydrazines , Pyrazoles , Spectrophotometry, Ultraviolet , Tablets , Pyrazoles/analysis , Pyrazoles/blood , Pyrazoles/chemistry , Benzoates/analysis , Benzoates/chemistry , Benzoates/blood , Hydrazines/analysis , Hydrazines/chemistry , Spectrophotometry, Ultraviolet/methods , Limit of Detection , Reproducibility of ResultsABSTRACT
Malondialdehyde (MDA) and formaldehyde (FA) are highly active carbonyl substances widely present in both biological and abiotic systems. The detection of MDA and FA is of great significance for disease diagnosis and food safety monitoring. However, due to the similarity in structural properties between MDA and FA, very few probes for synergistically detecting MDA and FA were reported. In addition, functional abnormalities in the Golgi apparatus are closely related to MDA and FA, but currently there are no fluorescent probes that can detect MDA and FA in the Golgi apparatus. Therefore, we constructed a simple Golgi-targetable fluorescent probe GHA based on hydrazine moiety as the recognition site to produce a pyrazole structure after reaction with MDA and to generate a CN double bond after reaction with FA, allowing MDA and FA to be distinguished due to different emission wavelengths during the recognition process. The probe GHA has good specificity and sensitivity. Under the excitation of 350 nm, the blue fluorescence was significantly enhanced at 424 nm when the probe reacted with MDA, and the detection limit was 71 nM. At the same time, under the same excitation of 350 nm, the reaction with FA showed a significant enhancement of green fluorescence at 520 nm, with a detection limit of 12 nM for FA. And the simultaneous and high-resolution imaging of MDA and FA in the Golgi apparatus of cells was achieved. In addition, the applications of the probe GHA in food demonstrated it can provide a powerful method for food safety monitoring. In summary, this study offers a promising tool for the synergistic identification and determination of MDA and FA in the biosystem and food, facilitating the revelation of their detailed functions in Golgi apparatus and the monitoring of food safety.
Subject(s)
Fluorescent Dyes , Formaldehyde , Golgi Apparatus , Malondialdehyde , Formaldehyde/chemistry , Formaldehyde/analysis , Golgi Apparatus/chemistry , Golgi Apparatus/metabolism , Fluorescent Dyes/chemistry , Humans , Malondialdehyde/analysis , Malondialdehyde/chemistry , Limit of Detection , Food Analysis/methods , HeLa Cells , Optical Imaging , Hydrazines/chemistry , Hydrazines/analysis , Food Contamination/analysisABSTRACT
ß-propiolactone (BPL) is an alkylating agent used for inactivation of biological samples such as vaccines. Due to its known carcinogenic properties, complete hydrolysis of BPL is essential, and the detection of trace amounts is crucial. In this study a novel High-Performance Liquid Chromatography-Ultraviolet (HPLC-UV) method was developed. Rhodamine B hydrazide (RBH) was synthesized and utilized as a derivatizing reagent to react with BPL. The reaction was optimized in a weak acidic solution, resulting in a high yield. The separation of the RBH-derivatized BPL was achieved on a C8 column and detected by a UV detector at a wavelength of 560 nm. The method's validation demonstrated a high linearity (r2 > 0.99) over a concentration range of 0.5-50 µg/mL, with detection and quantification limits of 0.17 µg/mL and 0.5 µg/mL, respectively. The average recovery of samples was 85.20 % with a relative standard deviation (RSD) of 1.75 %. This method was successfully applied for BPL residue analysis in inactivated COVID-19 vaccines. This novel derivatization method offers a promising solution for monitoring BPL residues in the vaccine production process for quality control purposes and compliance with regulatory standards.
Subject(s)
COVID-19 Vaccines , Limit of Detection , Propiolactone , Rhodamines , Chromatography, High Pressure Liquid/methods , Propiolactone/chemistry , Rhodamines/chemistry , Reproducibility of Results , COVID-19 Vaccines/chemistry , Vaccines, Inactivated/chemistry , Vaccines, Inactivated/analysis , Linear Models , SARS-CoV-2/chemistry , Humans , Hydrazines/chemistry , Hydrazines/analysisABSTRACT
Pesticide active ingredients are frequently detected in the rivers, creeks, wetlands, estuaries, and marine waters of the Great Barrier Reef (GBR) region and are one of the main contributors to poor water quality. Pesticide concentrations detected in the environment through water quality monitoring programs can be compared against estimates of ecologically "safe" concentrations (i.e., water quality guidelines) to assess the potential hazard and risk posed to aquatic ecosystems. Water quality guidelines are also required to estimate the aquatic risk posed by pesticide mixtures, which is used for the Reef 2050 Water Quality Improvement Plan pesticide target. Seventy-four pesticide active ingredients and their degradates are frequently detected in GBR catchment waterways, however many do not have water quality guidelines in the Australian and New Zealand Guidelines for Fresh and Marine Water Quality. The current study derives ecotoxicity threshold values (ETVs) as unendorsed guideline values for active ingredients in two fungicides (4-hydroxychlorothalonil (fungicide degradate) and carbendazim) and two insecticides (dimethoate and methoxyfenozide) that are commonly detected in GBR catchment waterways. The proposed ETVs have been derived using species sensitivity distributions, as recommended in the Australian and New Zealand nationally endorsed method for deriving water quality guidelines for aquatic ecosystem protection. Four ETVs were derived for each chemical with values that should theoretically protect 99, 95, 90 and 80 % of species (i.e., PC99, PC95, PC90, PC80, respectively). The PC99 and PC95 values for 4-hydroxychlorothalonil, carbendazim, dimethoate and methoxyfenozide were 0.49 µg/L and 4 µg/L, 0.029 µg/L and 0.45 µg/L, 0.11 µg/L and 5.8 µg/L and 0.19 µg/L and 2 µg/L, respectively. The ETVs will be used in an ecological hazard and risk assessment across GBR waterways in part two of this study. The ETVs can also be used to assess potential risk across Australia and internationally where monitoring data are available.
Subject(s)
Carbamates , Environmental Monitoring , Water Pollutants, Chemical , Water Pollutants, Chemical/analysis , Water Pollutants, Chemical/toxicity , Carbamates/toxicity , Carbamates/analysis , Seawater/chemistry , Fresh Water/chemistry , Australia , Insecticides/analysis , Insecticides/toxicity , Fungicides, Industrial/analysis , Fungicides, Industrial/toxicity , New Zealand , Pesticides/analysis , Pesticides/toxicity , Risk Assessment , Hydrazines/toxicity , Hydrazines/analysis , BenzimidazolesABSTRACT
Hydrazine (N2H4) and bisulfite (HSO3-) detection methods are urgently needed due to its harmful to the human health and environment safety. Herein, we reported a dual-response fluorescence probe EPC, which is capable of sequential detection of N2H4 and HSO3- by two different fluorescence signals. The probe EPC itself showed yellow florescence. In presence of N2H4, probe EPC exhibited an obviously fluorescence change (from yellow to green). However, a new addition product came into being after probe EPC mixed with HSO3-, followed with weak yellow emission. More important, probe EPC exhibited excellent fluorescence response properties for N2H4 and HSO3-, such as high sensitivity (0.182 µM for N2H4, 0.093 µM for HSO3-), rapid response (55 s for N2H4, 45 s for HSO3-), excellent selectivity and anti-interference performance. The sensing mechanisms for N2H4 and HSO3- were proved by 1H NMR and MS spectra. Practical applications were studied. EPC based test paper can be utilized for quantitative detecting N2H4 in actual water samples. And, probe EPC has been successfully applied to recognize N2H4 contaminant in soil samples. Moreover, EPC has great potential to be used to detect HSO3- in real food samples.
Subject(s)
Fluorescent Dyes , Hydrazines , Spectrometry, Fluorescence , Sulfites , Hydrazines/analysis , Hydrazines/chemistry , Fluorescent Dyes/chemistry , Spectrometry, Fluorescence/methods , Sulfites/analysis , Imidazoles/chemistry , Limit of DetectionABSTRACT
This work reports the development of novel curcuminoid-based electrochemical sensors for the detection of environmental pollutants from water. In this study, the first set of electrochemical experiments was carried out using curcumin-conjugated multi-walled carbon nanotubes (MWCNT-CM) for 1,4-dioxane detection. The MWCNT-CM/GCE showed good sensitivity (103.25 nA nM-1 cm-2 in the linear range 1 nM to 1 µM), with LOD of 35.71 pM and LOQ of 108.21 pM. The second set of electrochemical experiments was carried out with bisdemethoxy curcumin analog quantum dots (BDMCAQD) for hydrazine detection. The BDMCAQD/GCE exhibited good sensitivity (74.96 nA nM-1 cm-2 in the linear range 100 nM to 1 µM), with LOD of 10 nM and LOQ of 44.93 nM. Thus, this work will serve as a reference for the fabrication of metal-free electrochemical sensors using curcuminoids as the redox mediator for the enhanced detection of environmental pollutants.
Subject(s)
Curcumin , Electrochemical Techniques , Hydrazines , Nanotubes, Carbon , Hydrazines/analysis , Curcumin/analysis , Nanotubes, Carbon/chemistry , Dioxanes , Biosensing Techniques , Environmental Pollutants/analysis , Quantum Dots , Limit of Detection , Water Pollutants, Chemical/analysisABSTRACT
Hydrazine (N2H4), a crucial chemical raw material, enhances people's lives and fosters human progress. Hydrazine usage or leakage has caused environmental contamination, affecting water, soil, and living beings. Hydrazine simultaneously presents a possible risk to human health due to its carcinogenic properties. Thus, quick and precise detection of hydrazine is crucial in environmental studies and biological contexts. We prepared a red-emitting fluorescence turn-on probe (XT-HZ) to detect hydrazine specifically. The probe has a low detecting limit for hydrazine (63 nM) with excitation wavelength at 570 nm and emission wavelength at 625 nm. Besides, the probe XT-HZ had excellent water solubility, high selectivity, and good sensitivity for detecting hydrazine. Finally, probe XT-HZ was applied in the imaging of N2H4 in living cells, zebrafish and environmental water samples.
Subject(s)
Environmental Monitoring , Fluorescent Dyes , Hydrazines , Water Pollutants, Chemical , Hydrazines/analysis , Fluorescent Dyes/chemistry , Water Pollutants, Chemical/analysis , Environmental Monitoring/methods , Zebrafish , Animals , HumansABSTRACT
Thirty two commercially available standards were used to determine chromatographic retention indices for three different stationary phases (non-polar, polar and mid-polar) commonly used in gas chromatography. The selected compounds were nitrogen-containing heterocycles and amides, which are referred to in the literature as unsymmetrical dimethylhydrazine (UDMH) transformation products or its assumed transformation products. UDMH is a highly toxic compound widely used in the space industry. It is a reactive substance that forms a large number of different compounds in the environment. Well-known transformation products may exceed UDMH itself in their toxicity, but most of the products are poorly investigated, while posing a huge environmental threat. Experimental retention indices for the three stationary phases, retention indices from the NIST database, and predicted retention indices are presented in this paper. It is shown that there are virtually no retention indices for UDMH transformation products in the NIST database. In addition, even among those compounds for which retention indices were known, inconsistencies were identified. Adding retention indices to the database and eliminating erroneous data would allow for more reliable identification when standards are not available. The discrepancies identified between experimental retention index values and predicted values will allow for adjustments to the machine learning models that are used for prediction. Previously proposed compounds as possible transformation products without the use of standards and NMR method were confirmed.
Subject(s)
Machine Learning , Chromatography, Gas/methods , Hydrazines/analysis , Hydrazines/chemistry , Reproducibility of ResultsABSTRACT
Hydrogen sulfide (H2S) and hydrazine (N2H4) are toxic compounds in environmental and living systems, and hydrogen sulfide is also an important signaling molecule. However, in the absence of dual-color probes capable of detecting both H2S and N2H4, the ability to monitor the crosstalk of these substances is restricted. Herein, we developed an ESIPT-based dual-response fluorescent probe (BDM-DNP) for H2S and N2H4 detection via dually responsive sites. The BDM-DNP possessed absorbing strength in the detection of H2S and N2H4, with a large Stokes shift (156 nm for H2S and 108 nm for N2H4), high selectivity and sensitivity, and good biocompatibility. Furthermore, BDM-DNP can be utilized for the detection of hydrogen sulfide and hydrazine in actual soil, and gaseous H2S and N2H4 in environmental systems. Notably, BDM-DNP can detect H2S and N2H4 in living cells for disease diagnosis and treatment evaluation.
Subject(s)
Fluorescent Dyes , Hydrazines , Hydrogen Sulfide , Hydrogen Sulfide/analysis , Hydrazines/chemistry , Hydrazines/analysis , Fluorescent Dyes/chemistry , Humans , Molecular Structure , ColorABSTRACT
The increasing utilization of hydrazine and its derivatives across diverse sectors highlights the pressing need for efficient detection methods to safeguard human health and the environment. Likewise, nicardipine, a widely used medication for heart diseases, necessitates accurate sensing techniques for clinical research and therapeutic monitoring. Here, we propose a novel approach using a naphthalimide-functionalized Zr-MOF as a fluorometric probe capable of detecting both hydrazine and nicardipine in aqueous medium. Our designed probe exhibited a significant 31-fold increase in fluorescence intensity upon interaction with hydrazine. At the same time, nicardipine induced 86% fluorescence quenching with an exceptionally rapid response time (100 s for hydrazine and 5 s for nicardipine). The designed probe has the ability to detect both analytes at nanomolar concentrations (LOD for hydrazine is 1.11 nM while that for nicardipine is 9.6 nM). Investigation across various wastewater samples and pH conditions further validated its practical utility. The mechanism behind fluorometric sensing of nicardipine was thoroughly investigated using modern instrumentation. Our study presents a versatile and effective approach for detecting hydrazine and nicardipine, addressing crucial needs in both industrial and biomedical contexts.
Subject(s)
Antihypertensive Agents , Hydrazines , Metal-Organic Frameworks , Naphthalimides , Nicardipine , Hydrazines/analysis , Hydrazines/chemistry , Nicardipine/analysis , Naphthalimides/chemistry , Metal-Organic Frameworks/chemistry , Antihypertensive Agents/analysis , Fluorescent Dyes/chemistry , Molecular Structure , Spectrometry, FluorescenceABSTRACT
Extensive utilization of pesticides and herbicides to boost agricultural production increased the environmental health risks, which can be mitigate with the aid of highly sensitive detection systems. In this study, an electrochemical sensor for monitoring the carcinogenic pesticides in the environmental samples has been developed based on sulfur-doped graphitic-carbon nitride-gold nanoparticles (SCN-AuNPs) nanohybrid. Thermal polycondensation of melamine with thiourea followed by solvent exfoliation via ultrasonication leads to SCN formation and electroless deposition of AuNPs on SCN leads to SCN-AuNPs nanohybrid synthesis. The chemical composition, S-doping, and the morphology of the nanohybrid were confirmed by various microscopic and spectroscopic tools. The as-synthesized nanohybrid was fabricated with glassy carbon (GC) electrode for determining the carcinogenic hydrazine (HZ) and atrazine (ATZ) in field water samples. The present sensor exhibited superior electrocatalytic activity than GC/SCN and GC/AuNPs electrodes due to the synergism between SCN and AuNPs and the amperometric studies showed the good linear range of detection of 20 nM-0.5 mM and 500 nM-0.5 mM with the limit of detection of 0.22 and 69 nM (S/N = 3) and excellent sensitivity of 1173.5 and 13.96 µA mM-1 cm-2 towards HZ and ATZ, respectively. Ultimately, the present sensor is exploited in environmental samples for monitoring HZ and ATZ and the obtained results are validated with high-performance liquid chromatography (HPLC) technique. The excellent recovery percentage and close agreement with the results of HPLC analysis proved the practicability of the present sensor. In addition, the as-prepared materials were utilized for the photocatalytic degradation of ATZ and the SCN-AuNPs nanohybrid exhibited higher photocatalytic activity with the removal efficiency of 93.6% at 90 min. Finally, the degradation mechanism was investigated and discussed.
Subject(s)
Carcinogens , Gold , Graphite , Metal Nanoparticles , Water Pollutants, Chemical , Gold/chemistry , Water Pollutants, Chemical/analysis , Water Pollutants, Chemical/chemistry , Metal Nanoparticles/chemistry , Graphite/chemistry , Carcinogens/analysis , Atrazine/analysis , Atrazine/chemistry , Sulfur/chemistry , Sulfur/analysis , Electrochemical Techniques/methods , Hydrazines/analysis , Hydrazines/chemistry , Nitrogen Compounds/chemistry , Nitrogen Compounds/analysis , Nitriles/chemistry , Nitriles/analysis , Environmental Monitoring/methodsABSTRACT
BACKGROUND: Hydrazine (N2H4) is a highly toxic and versatile chemical raw material, which poses a serious threat to the environment and human health when used in large quantities. However, the traditional methods for the detection of N2H4 have the disadvantages of time-consuming, complicated operation and expensive instruments. In contrast, fluorescence probes have many advantages, such as simple operation, high sensitivity, good selectivity, and fast response time. Therefore, there is an urgent need for a fluorescence probe that can rapidly and accurately detect the presence of N2H4 and monitor the changes in its concentration. RESULTS: For this purpose, we designed and synthesized a series of myricetin fluorescence probes 3-(substituent group)-5,7-dimethoxy-4-oxo-2-(3,4,5-trimethoxy. phenyl)-4H-chromen-4-one (Myr-R) for N2H4 detection. In the presence of N2H4, the probe 5,7-dimethoxy-3-(2,3,4,5,6-pentafluorobenzoate)-2-(3,4,5-trimethoxyphen-yl). -4H-chr-omen-4-one (Myr-3) shows significant fluorescence changes, double emission properties and a large Stokes shift (183 nm), and exhibits high selectivity and sensitivity to N2H4 (The detection limit is 93 nM). Importantly, the qualitative and quantitative analysis of N2H4 in water, soil, and air can be accomplished using fluorescence, smartphone, and UV lamps coupled with Myr-3. In addition, Myr-3 can be used for monitoring and imaging intracellular N2H4. Meanwhile, the fluorophore 3-hydroxy-5,7-dimethoxy-2-(3,4,5-trimethoxyphenyl)-4H-benzopyran-4-one (Myr-Me) was applied to fingerprinting of different substrate materials due to the fact that it exhibits strong yellow fluorescence emission in the solid state and shows excellent contrast and high resolution. SIGNIFICANCE: The probe Myr-3 is not only able to rapidly detect N2H4 in complex environments, but also can be used for imaging intracellular N2H4. In addition, the fluorophore Myr-Me can be used as an effective imaging agent for visual fingerprinting. These properties enable the probe Myr-3 and the fluorophore Myr-Me for a wide range of potential applications in related fields.
Subject(s)
Flavonoids , Water , Humans , HeLa Cells , Water/chemistry , Hydrazines/analysis , Fluorescent Dyes/chemistry , Spectrometry, Fluorescence/methodsABSTRACT
Hydrazine (N2H4) is an important industrial raw material that has been widely used in industrial production and agricultural interventions, but its widespread application also inevitably causes environmental pollution. In this study, based on resorufin, we constructed a novel "turn-on" fluorescent probe RFT for the selective detection of hydrazine under complex environmental conditions and in vivo. The probe RFT exhibited excellent stability and selectivity towards the detection of hydrazine with a low detection limit of 260 nM. In addition, RFT was successfully applied to the detection of hydrazine in environmental water samples and living cells. Most importantly, RFT could not only detect the exogenous hydrazine in zebrafish and mice, but also image and visualize the up-regulation of endogenous hydrazine induced by isoniazid in zebrafish.
Subject(s)
Fluorescent Dyes , Zebrafish , Mice , Animals , Spectrometry, Fluorescence/methods , Hydrazines/analysisABSTRACT
Hydrazine (N2H4) plays an important role in industrial production, but it is highly toxic, leaking or exposing it will pollute the environment and cause serious harm to human beings. Therefore, it is necessary to use a simple and effective method to detect N2H4 in environmental systems and organisms. Herein, a novel water-soluble fluorescent probe based on coumarin fluorophore, 2-(7-(diethylamino)-2-oxo-2H-chromen-3-yl)isoindoline-1,3-dione (C-Z1), is reported. The fluorescence intensity of the probe at 530 nm was enhanced gradually with the addition of N2H4, and the maximum enhancement was about 28 times. The probe has good selectivity and sensitivity, the detection limit of hydrazine hydrate is 1.48 × 10-7 M, and the response mechanism of the probe is proved by theoretical calculation and experiment. C-Z1 has been shown to detect N2H4 in a variety of environmental samples, including water, soil, air, cells, zebrafish and plants. In addition, C-Z1 can be made into test strips for easy portability and used for rapid quantitative detection of N2H4 in the field by its distinct change in fluorescence color. Thus, C-Z1 has great potential for the analysis and detection of environmental contaminants.
Subject(s)
Fluorescent Dyes , Zebrafish , Animals , Humans , Fluorescent Dyes/toxicity , Fluorescent Dyes/analysis , HeLa Cells , Water , Hydrazines/analysis , Spectrometry, Fluorescence , Plant Roots/chemistryABSTRACT
An acetoxy naphthaldehyde conjugated benzophenoxazinium chloride chromophore-based-donor-π-acceptor (D-π-A) fluorescent probe BPN (benzophenoxazinium naphthoxy imine) displaying near-infrared (NIR) emission was reported for hydrazine detection. The chosen water-soluble benzophenoxazinium chloride chromophore has excellent photostability, a high molar extinction coefficient and fluorescence quantum yield (Φ = from 0.0075 to 0.6193), higher selectivity towards hydrazine and a longer fluorescence lifetime. In the presence of hydrazine, BPN exhibits near infrared fluorescence emission at 725 nm along with color change from light blue to red, as detected by the naked eye. Moreover, the BPN probe can selectively detect hydrazine (DL = 4.5 × 10-10 M) in a 90% aqueous DMSO solution without interfering with other analytes. As proof of real samples, the probe is successfully applied to sense hydrazine in thin layer chromatography (TLC) paper strips (both solution and vapor phases) and water and soil samples, suggesting its significant potential application. Also, due to its NIR emission and aqueous solubility, the BPN probe can be successfully used in live cell imaging with low cytotoxicity.
Subject(s)
Chlorides , Fluorescent Dyes , Fluorescent Dyes/chemistry , Spectrometry, Fluorescence/methods , Hydrazines/analysis , WaterABSTRACT
The microenvironments of biological systems are associated with the pathology of organisms. This study, aimed to construct a hemicyanine-based probe (1), which can respond to mitochondrial viscosity and hydrazine (N2H4), for imaging application in living cells and zebrafish. The probe showed no fluorescence due to the intramolecular rotation in the solution; however, it exhibited a strong emission at 730 nm when the molecules were restricted to a high-viscosity environment. The addition of N2H4 caused an elimination reaction of the N-substituted group in the pyridinium part and further broke the CC bond to produce a highly fluorescent hydrazone. Also, the probe could selectively and quantitatively detect N2H4 via the fluorescence enhancement at 510 nm in a concentration range of 0 µM-140µM, with the limit of detection being 0.0485 µM. This probe may be used to study diseases related to N2H4 and viscosity changes in biological systems. Furthermore, the analysis methods based on probe 1 for N2H4 detection in soil, water, and air samples were successfully established.
Subject(s)
Fluorescent Dyes , Zebrafish , Humans , Animals , Fluorescent Dyes/chemistry , Viscosity , Water/chemistry , Hydrazines/analysis , HeLa Cells , Spectrometry, Fluorescence/methodsABSTRACT
Hydrazine (N2H4) is a significant chemical reagent and widely applied in industrial field, which can bring potential risk to environmental safety and human health due to its high toxicity and potential carcinogenicity. In this paper, a flavonol-derived fluorescent probe named TB-N2H4 was rationally developed for detecting N2H4 based on the excited intramolecular proton transfer (ESIPT) principle. TB-N2H4 exhibited a remarkable fluorescence turn-on response toward N2H4 with a large Stokes shift of 191 nm. Moreover, TB-N2H4 could selectively recognize N2H4 over other competitive analytes, and displayed high sensitivity toward N2H4 with a low detection limit of 0.117 µM. The sensing mechanism of the probe TB-N2H4 for N2H4 was confirmed by theoretical calculation and HRMS analysis. This probe was able to quantitatively determine N2H4 in environmental water and soil samples. Additionally, TB-N2H4 was also successfully utilized for real-time tracking of the distribution of N2H4 in living zebrafish.
Subject(s)
Fluorescent Dyes , Zebrafish , Animals , Humans , Fluorescent Dyes/chemistry , Spectrometry, Fluorescence , Protons , Hydrazines/analysis , HeLa CellsABSTRACT
Carcinogenic N-nitrosamines were recently found in the sartan family of drugs and caused many drug recalls. Both of their detection and quantification are therefore important. Methods reported for N-nitrosamine quantitation rely on the use of standards and are just applicable to simple N-nitrosamines. There is an urgent need to quantify N-nitrosamines derived from drugs with a complicated structure that lack standards. To tackle the issue, this study describes a novel absolute quantitation strategy for N-nitrosamines using coulometric mass spectrometry (CMS) without standards. In our approach, N-nitrosamine is first converted into electrochemically active hydrazine via zinc reduction under acidic condition and the resulting hydrazine can then be easily quantified using CMS. To validate our method, six simple N-nitrosamines, N-nitrosodiethylamine (NDEA), N-nitroso-4-phenylpiperidine (NPhPIP), N-nitrosodiphenylamine (NDPhA), N-nitrosodibutylamine (NDBA), N-nitrosodipropylamine (NDPA), and N-nitrosopiperidine (NPIP), were chosen as test samples, and they all were quantified with excellent measurement accuracy (quantitation error ≤1.1%). Taking this one step further, as a demonstration of the method utility, a drug-like N-nitrosamine, (R)-N-(2-(6-chloro-5-methyl-1'-nitroso-2,3-dihydrospiro[indene-1,4'-piperidin]-3-yl)propan-2-yl)acetamide (VII), was also synthesized and successfully quantified using our method at 15 ppb level in a complex formulation matrix, following solvent extraction, N-nitrosamine isolation, and reductive conversion. Because of the feature of requiring no standards, CMS provides a simple and powerful approach for N-nitrosamine absolute quantitation and has great potential for analysis of other drug impurities or metabolites.
Subject(s)
Nitrosamines , Gas Chromatography-Mass Spectrometry/methods , Hydrazines/analysis , Nitrosamines/analysis , Tandem Mass SpectrometryABSTRACT
The dissipation, conversion and risk assessment of bifenazate and bifenazate-diazene in garlic plant were studied by a modified QuEChERS method coupled with UHPLC-MS/MS for the first time. Bifenazate dissipated rapidly in garlic chive and serpent garlic with the half-lives of 3.0-3.9 days and 6.1-6.9 days, respectively. Bifenazate residue on garlic (<0.01 mg/kg) was significantly lower than the other two matrices in the whole growing period, which meant residues in the above-ground part were not transferred to the garlic. Furthermore, garlic chive had higher residues than serpent garlic due to the differences in morphological characteristics. Bifenazate-diazene was easier to convert to bifenazate, with the conversion rates of 93%, 16% and 32% in garlic, serpent garlic and garlic chive extracts, respectively. Additionally, the dietary intake risk for bifenazate was acceptable with RQchronic < 100% according to the international and national assessments.
Subject(s)
Carbamates/analysis , Garlic , Hydrazines/analysis , Pesticide Residues/analysis , Food Analysis , Garlic/chemistry , Risk Assessment , Tandem Mass SpectrometryABSTRACT
The rapid and sensitive detection of plant-growth-regulator (PGR) residue is essential for ensuring food safety for consumers. However, there are many disadvantages in current approaches to detecting PGR residue. In this paper, we demonstrate a highly sensitive PGR detection method by using terahertz time-domain spectroscopy combined with metamaterials. We propose a double formant metamaterial resonator based on a split-ring structure with titanium-gold nanostructure. The metamaterial resonator is a split-ring structure composed of a titanium-gold nanostructure based on polyimide film as the substrate. Also, terahertz spectral response and electric field distribution of metamaterials under different analyte thickness and refractive index were investigated. The simulation results showed that the theoretical sensitivity of resonance peak 1 and peak 2 of the refractive index sensor based on our designed metamaterial resonator approaches 780 and 720 gigahertz per refractive index unit (GHz/RIU), respectively. In experiments, a rapid solution analysis platform based on the double formant metamaterial resonator was set up and PGR residues in aqueous solution were directly and rapidly detected through terahertz time-domain spectroscopy. The results showed that metamaterials can successfully detect butylhydrazine and N-N diglycine at a concentration as low as 0.05 mg/L. This study paves a new way for sensitive, rapid, low-cost detection of PGRs. It also means that the double formant metamaterial resonator has significant potential for other applications in terahertz sensing.