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1.
J Sep Sci ; 47(2): e2300757, 2024 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-38286731

RESUMO

A new green micellar liquid chromatographic method has been developed and validated for the simultaneous determination of diphenhydramine (DPH) and tripelennamine hydrochloride (TRP) using a micellar mobile phase consisting of 1 mM Tween 20 in phosphate buffer pH 4:isopropanol (85:15, %v/v). The method was linear in the range of 4-150 and 5-120 µg/mL for TRP and DPH, respectively. The method was successfully applied for the simultaneous determination of DPH and TRP in a laboratory-prepared gel containing all possible excipients with mean percent recoveries ± standard deviation of 100.346 ± 1.265 and 100.754 ± 1.117 for TRP and DPH, respectively. The method was validated according to the International Conference on Harmonization guidelines. The method is confirmed to have excellent greenness.


Assuntos
Difenidramina , Tripelenamina , Difenidramina/análise , Micelas , Cromatografia Líquida/métodos , Indicadores e Reagentes , Cromatografia Líquida de Alta Pressão/métodos
2.
Luminescence ; 39(7): e4815, 2024 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-38972855

RESUMO

A green micellar synchronous spectrofluorimetric method was developed and validated for simultaneous determination of tripelennamine hydrochloride and diphenhydramine in bulk and combined pharmaceutical formulation. Synchronous fluorescence of tripelennamine hydrochloride and diphenhydramine was determined using Δλ = 60 nm. The first derivative of synchronous fluorescence was computed to resolve overlap in the synchronous fluorescence spectra. Tripelennamine hydrochloride was quantified at 375 nm, whereas diphenhydramine was quantified at 293 nm; each is the zero-crossing point of the other. As diphenhydramine exhibited weak native fluorescence, micelle enhancement upon incorporation of sodium dodecyl sulfate was considered. Two-level full factorial design was carried out to optimize experimental parameters. Optimum conditions involved using SDS (2% w/v) along with Teorell and Stenhagen buffer (pH 9). The method was found to be linear over the range 0.2-4.5 and 0.2-5 µg/mL for tripelennamine and diphenhydramine, respectively, with limits of detection 0.211 and 0.159 µg/mL. The method was successfully applied for simultaneous determination of tripelennamine hydrochloride and diphenhydramine in laboratory-prepared gel containing all possible excipients with mean percent recoveries ±SD 100.59 ± 0.79 and 98.99 ± 0.98 for tripelennamine hydrochloride and diphenhydramine, respectively. The proposed method was proved to be eco-friendly using different greenness assessment tools.


Assuntos
Difenidramina , Micelas , Espectrometria de Fluorescência , Difenidramina/análise , Difenidramina/química , Espectrometria de Fluorescência/métodos , Géis/química , Dodecilsulfato de Sódio/química , Concentração de Íons de Hidrogênio
3.
Opt Express ; 29(16): 24723-24734, 2021 Aug 02.
Artigo em Inglês | MEDLINE | ID: mdl-34614822

RESUMO

'Molecular fingerprinting' with Raman spectroscopy can address important problems-from ensuring our food safety, detecting dangerous substances, to supporting disease diagnosis and management. However, the broad adoption of Raman spectroscopy demands low-cost, portable instruments that are sensitive and use lasers that are safe for human eye and skin. This is currently not possible with existing Raman spectroscopy approaches. Portability has been achieved with dispersive Raman spectrometers, however, fundamental entropic limits to light collection both limits sensitivity and demands high-power lasers and cooled expensive detectors. Here, we demonstrate a swept-source Raman spectrometer that improves light collection efficiency by up to 1000× compared to portable dispersive spectrometers. We demonstrate high detection sensitivity with only 1.5 mW average excitation power and an uncooled amplified silicon photodiode. The low optical power requirement allowed us to utilize miniature chip-scale MEMS-tunable lasers with close to eye-safe optical powers for excitation. We characterize the dynamic range and spectral characteristics of this Raman spectrometer in detail, and use it for fingerprinting of different molecular species consumed everyday including analgesic tablets, nutrients in vegetables, and contaminated alcohol. By moving the complexity of Raman spectroscopy from bulky spectrometers to chip-scale light sources, and by replacing expensive cooled detectors with low-cost uncooled alternatives, this swept-source Raman spectroscopy technique could make molecular fingerprinting more accessible.


Assuntos
Lentes , Dispositivos Ópticos , Análise Espectral Raman/instrumentação , Acetaminofen/análise , Bebidas Alcoólicas/análise , Difenidramina/análise , Desenho de Equipamento , Humanos , Ibuprofeno/análise , Ibuprofeno/química , Lasers , Metanol/análise , Nutrientes/análise , Análise Espectral Raman/métodos , Tolueno/análise , Verduras/química
4.
Luminescence ; 35(4): 550-560, 2020 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-31904176

RESUMO

Simple and rapid synchronous fluorometric methods were adopted and validated for the simultaneous analysis of a binary mixture of diphenhydramine (DIP) and ibuprofen (IBU) (Mix I) or DIP and phenylephrine (PHE) (Mix II) in their co-formulated pharmaceuticals without prior separation. Analysis of Mix I is based on the measurement of the peak amplitudes (D1 ) of synchronous fluorescence intensities at 265.1 nm for DIP and 260 nm for IBU. The relationship between the concentration and the amplitude of the first-derivative synchronous fluorescence spectra showed good linearity over the concentration ranges 0.50-10.00 µg ml-1 and 0.50-7.90 µg ml-1 for DIP and IBU, respectively. Analysis of Mix II was based on measurement of the peak amplitude (D1 ) synchronous fluorescence intensities at 230 nm for DIP and at 253.9 nm for PHE. Moreover, for Mix II, the peak amplitude (D2 ) synchronous fluorescence intensities were measured at 227.9 nm for DIP and at 264.9 nm for PHE. Calibration plots were rectilinear over the concentration range 0.30-3.50 µg ml-1 and 0.03-0.75 µg ml-1 for DIP and PHE, respectively. The proposed methods were successfully applied to determine the studied compounds in pure form and in pharmaceutical preparations.


Assuntos
Difenidramina/análise , Ibuprofeno/análise , Fenilefrina/análise , Calibragem , Estrutura Molecular , Espectrometria de Fluorescência
5.
Acta Pol Pharm ; 71(5): 721-9, 2014.
Artigo em Inglês | MEDLINE | ID: mdl-25362800

RESUMO

Diphenhydramine hydrochloride (DPH), a histamine H1-receptor antagonist, is widely used as antiallergic, antiemetic and antitussive drug found in many pharmaceutical preparations. In this study, a new reconstitutable syrup formulation of DPH was prepared because it is more stable in solid form than that in liquid form. The quantitative estimation of the DPH content of a reconstitutable syrup formulation in the presence of pharmaceutical excipients, D-sorbitol, sodium citrate, sodium benzoate and sodium EDTA is not possible by the direct absorbance measurement. Therefore, a signal processing approach based on continuous wavelet transform was used to determine the DPH in the reconstitutable syrup formulations and to eliminate the effect of excipients on the analysis. The absorption spectra of DPH in the range of 5.0-40.0 µg/mL were recorded between 200-300 nm. Various wavelet families were tested and Biorthogonal1.1 continuous wavelet transform (BIOR1.1-CWT) was found to be optimal signal processing family to get fast and desirable determination results and to overcome excipient interference effects. For a comparison of the experimental results obtained by partial least squares (PLS) and principal component regression (PCR) methods were applied to the quantitative prediction of DPH in the mentioned samples. The validity of the proposed BIOR1.1-CWT, PLS and PCR methods were achieved analyzing the prepared samples containing the mentioned excipients and using standard addition technique. It was observed that the proposed graphical and numerical approaches are suitable for the quantitative analysis of DPH in samples including excipients.


Assuntos
Difenidramina/análise , Antagonistas dos Receptores Histamínicos H1/análise , Processamento de Sinais Assistido por Computador , Espectrofotometria Ultravioleta , Calibragem , Química Farmacêutica , Excipientes/análise , Análise dos Mínimos Quadrados , Soluções Farmacêuticas , Análise de Componente Principal , Padrões de Referência , Reprodutibilidade dos Testes , Espectrofotometria Ultravioleta/normas , Análise de Ondaletas
6.
Yao Xue Xue Bao ; 48(1): 94-7, 2013 Jan.
Artigo em Zh | MEDLINE | ID: mdl-23600148

RESUMO

This paper reports the establishment of a method for rapid identification 15 effective components of anti common cold medicine (paracetamol, aminophenazone, pseudoephedrine hydrochloride, methylephedrine hydrochloride, caffeine, amantadine hydrochloride, phenazone, guaifenesin, chlorphenamine maleate, dextromethorphen hydrobromide, diphenhydramine hydrochloride, promethazine hydrochloride, propyphenazone, benorilate and diclofenac sodium) with MRM by LC-MS/MS. The samples were extracted by methanol and were separated from a Altantis T3 column within 15 min with a gradient of acetonitrile-ammonium acetate (containing 0.25% glacial acetic acid), a tandem quadrupole mass spectrometer equipped with electrospray ionization source (ESI) was used in positive ion mode, and multiple reaction monitoring (MRM) was performed for qualitative analysis of these compounds. The minimum detectable quantity were 0.33-2.5 microg x kg(-1) of the 15 compounds. The method is simple, accurate and with good reproducibility for rapid identification many components in the same chromatographic condition, and provides a reference for qualitative analysis illegally added chemicals in anti common cold medicine.


Assuntos
Anti-Inflamatórios não Esteroides/análise , Antipiréticos/análise , Acetaminofen/análise , Acetanilidas/análise , Amantadina/análise , Aminopirina/análise , Antipirina/análogos & derivados , Antipirina/análise , Cafeína/análise , Clorfeniramina/análise , Cromatografia Líquida , Diclofenaco/análise , Difenidramina/análise , Contaminação de Medicamentos , Estabilidade de Medicamentos , Efedrina/análogos & derivados , Efedrina/análise , Guaifenesina/análise , Prometazina/análise , Pseudoefedrina/análise , Reprodutibilidade dos Testes , Salicilatos/análise , Espectrometria de Massas por Ionização por Electrospray , Espectrometria de Massas em Tandem
7.
Sci Total Environ ; 855: 158982, 2023 Jan 10.
Artigo em Inglês | MEDLINE | ID: mdl-36155033

RESUMO

With rapid economic development, an increasing number of people suffer from mental health diseases, which are gradually receiving the attention of society. However, basic data from surveys of mental disorders are limited. Composite influent samples were collected from 26 wastewater treatment plants in 23 major cities in China. The concentrations of the psychoactive drugs diphenhydramine, fluoxetine, doxepin, imipramine, sulpiride, zolpidem, carbamazepine, and flunitrazepam in the wastewater were determined. The detection frequency of diphenhydramine, sulpiride, and carbamazepine was close to 100 %, whereas that of the compounds was lower than 35 %. Carbamazepine had the highest mean consumption (31.1 mg/d/1000 people), followed by diphenhydramine (10.4 mg/d/1000 people) and sulpiride (11.3 mg/d/1000 people). Wastewater-based epidemiology (WBE) estimates of the average use of the three drugs were lower than those from the drug statistics data. Consumption of diphenhydramine in northern China was higher than that in southern China. A correlation analysis of psychotropic and illicit drugs revealed a correlation between sulpiride and heroin use, which may be related to the adverse effects of sulpiride treatment after heroin withdrawal. Psychotropic drug use is associated with both economic and social factors. We found associations between the use of the three drugs and age, occupation, and obesity, which are risk factors for mental disorders. The results showed that the monitoring of psychotropic drug using WBE has a certain reference value for public health care and for improving the understanding of mental disorders.


Assuntos
Vigilância Epidemiológica Baseada em Águas Residuárias , Poluentes Químicos da Água , Humanos , Cidades , Heroína/análise , Sulpirida/análise , Poluentes Químicos da Água/análise , Águas Residuárias/análise , Psicotrópicos/análise , China/epidemiologia , Carbamazepina/análise , Difenidramina/análise
8.
Analyst ; 135(6): 1259-67, 2010 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-20498877

RESUMO

Aerosol drugs dominate a significant share of pharmaceutical preparations on the market. A novel sensitive method utilizing nano extractive electrospray ionization mass spectrometry (nanoEESI-MS) has been developed for the rapid analysis of aerosol drug samples with quantitative information. Without any sample pretreatment, aerosol drugs were manually sprayed into the primary ion plume created by a nano electrospray emitter for direct ionization under ambient conditions. The analyte ions of interest were guided into an ion trap mass spectrometer for tandem mass analysis. The active ingredients of various aerosol drugs, such as econazole nitrate, beclomethasone dipropionate, binary mixture of methyl salicylate and diphenhydramine, terbutaline, and salbutamol, were rapidly detected using nanoEESI-MS. A single sample analysis could be completed within 1.2 s. Tandem mass spectrometry was used to confirm the identification of important compounds in each aerosol drug sample. Reasonable relative standard deviation (RSD = 6.39%, n = 13) and acceptable sensitivity (10 ppt, 100 muL) were found for the salbutamol aerosol sample, which suggests that nanoEESI-MS has the quantitative capacity for analyzing complex pharmaceutical samples. This method was further extended to study the thermal decomposition process of salbutamol, showing that the degradation kinetics of salbutamol can be conveniently tracked. Our data demonstrate that nanoEESI tandem mass spectrometry is a fast and sensitive technique for the analysis of aerosol drug preparations, showing promising applications in pharmacology studies and in situ analysis of aerosol drugs on the market.


Assuntos
Gases/química , Preparações Farmacêuticas/química , Espectrometria de Massas por Ionização por Electrospray/métodos , Agonistas Adrenérgicos beta/análise , Albuterol/análise , Antialérgicos/análise , Anti-Inflamatórios/análise , Antifúngicos/análise , Antirreumáticos/análise , Beclometasona/análise , Difenidramina/análise , Econazol/análise , Nanotecnologia , Salicilatos/análise , Espectrometria de Massas por Ionização por Electrospray/instrumentação , Espectrometria de Massas em Tandem , Terbutalina/análise
9.
Arch Environ Contam Toxicol ; 59(3): 343-51, 2010 Oct.
Artigo em Inglês | MEDLINE | ID: mdl-20340015

RESUMO

Biosolids land application is an important pathway introducing pharmaceuticals into the environment. In this work, laboratory column and dissipation experiments were performed using soils of varying properties in order to study the fate and transport of pharmaceutical residues introduced by the land application of biosolids. For experimentation, five pharmaceutical compounds (carbamazepine, diphenhydramine, fluoxetine, diltiazem, and clindamycin) and two metabolites (carbamazepine-10,11-epoxide and norfluoxetine) commonly found in biosolids were selected. Leaching experiments indicate that the selected pharmaceuticals have low mobility in tested soils. However, small portions of the applied pharmaceuticals were recovered in the leachates, likely attributed to sorption to dissolved organic matter. Dissipation experiments show that carbamazepine, diphenhydramine, and fluoxetine were persistent in soils, whereas the dissipation of diltiazem and clindamycin was affected by redox conditions and soil properties.


Assuntos
Recuperação e Remediação Ambiental/métodos , Preparações Farmacêuticas/química , Poluentes do Solo/química , Carbamazepina/análise , Carbamazepina/química , Clindamicina/análise , Clindamicina/química , Diltiazem/análise , Diltiazem/química , Difenidramina/análise , Difenidramina/química , Fluoxetina/análise , Fluoxetina/química , Preparações Farmacêuticas/análise , Esgotos/química , Poluentes do Solo/análise
10.
Zhongguo Zhong Yao Za Zhi ; 35(21): 2838-41, 2010 Nov.
Artigo em Zh | MEDLINE | ID: mdl-21322943

RESUMO

OBJECTIVE: To establish RP-HPLC method for determination of atropine sulphate, diphenhydramine hydrochloride, capsaicin and dihydrocapsaicin in pain-relieving plaster for arthritis. METHOD: The sample were separated on an Alltima C18 Column (4.6 mm x 250 mm, 5 microm) with the moblie phase of CH3 CN-0.1% H3 PO4. Flow rate was 1 mL x min(-1). The detective wavelength was set at 210 and 280 nm. Column temperature was 30 degrees C. RESULT: The calibration curve for atropine sulphate, diphenhydramine hydrochloride, capsaicin and dihydrocapsaicin revealed linearity in the range of 2.01-50.25, 15.08-377.00, 5.02-125.50, 5.03-125.75 mg x L(-1), respectively. The recoveries of atropine sulphate, diphenhydramine hydrochloride, capsaicin and dihydrocapsaicin were 99.00% with RSD of 0.95%, 99.89% with RSD of 1.2%, 100.1% with RSD of 1.5% and 99.51%, with RSD of 1.4%, respectively. CONCLUSION: The method is simple, rapid and accurate, which is suitable for the quality control of pain-relieving plaster for arthritis.


Assuntos
Artrite/tratamento farmacológico , Atropina/análise , Capsaicina/análogos & derivados , Capsaicina/análise , Cromatografia Líquida de Alta Pressão/métodos , Difenidramina/análise , Medicamentos de Ervas Chinesas/análise , Dor/tratamento farmacológico , Atropina/uso terapêutico , Capsaicina/uso terapêutico , Difenidramina/uso terapêutico , Medicamentos de Ervas Chinesas/uso terapêutico , Humanos
11.
Spectrochim Acta A Mol Biomol Spectrosc ; 233: 118213, 2020 Jun 05.
Artigo em Inglês | MEDLINE | ID: mdl-32169799

RESUMO

Two new smart spectrophotometric methods are developed and validated for the determination of the quatertnary mixture of paracetamol (acetaminophen), diphenhydramine, p-aminophenol, and N-oxide degradate of diphenhydramine. Method A is the novel triple divisor ratio difference method, where the triple divisor ratio spectrum of the component of interest shows a significant amplitude difference at two selected wavelengths where the three interfering substances are used as triple divisor and give constant amplitude all over the spectrum. The triple divisors are normalized spectra of tertiary mixtures containing 40 µg/mL of each of the 3 interfering components. The selected wavelengths are 256-290 nm, 220-230 nm, 230-245 nm and 275-260 nm for the 4 components, respectively. Method B is double divisor - ratio difference-dual wavelength, where the double divisor ratio spectrum of the component of interest shows a significant amplitude difference at two selected wavelengths where two interfering substances are used as double divisor and give constant amplitude all over the spectrum, while the third one shows zero amplitude difference at these two selected wavelengths. The double divisors used are normalized spectra of diphenhydramine /N-oxide degradate of diphenhydramine binary mixture for both paracetamol and p-aminophenol and paracetamol/p-aminophenol binary mixture for both diphenhydramine hydrochloride and its N-oxide degradate. The double divisors binary mixtures contain 40 µg/mL of each component. The selected wavelengths are 243-233 nm, 223.8-270.2 nm, 237-250 nm and 265-234.6 nm for the 4 compounds, respectively. Both methods were successfully applied for the quantification of the four components in laboratory prepared quaternary mixtures and for the quantification of paracetamol and diphenhydramine hydrochloride in panadol night® tablets. The results obtained by the developed methods were compared with those obtained by the United State Pharmacopeial method for the analysis of paracetamol and diphenhydramine, where no significant differences were found.


Assuntos
Acetaminofen/análise , Aminofenóis/análise , Difenidramina/análise , Processamento de Sinais Assistido por Computador , Espectrofotometria Ultravioleta
12.
Water Res ; 43(6): 1766-74, 2009 Apr.
Artigo em Inglês | MEDLINE | ID: mdl-19232423

RESUMO

The degradation of four pharmaceutical compounds (PhACs), ibuprofen (IBU), diphenhydramine (DP), phenazone (PZ), and phenytoin (PHT) was investigated via ultraviolet (UV) photolysis and UV/H(2)O(2) process with a low-pressure (LP) UV lamp. For each PhAC tested, direct photolysis quantum yields at 254 nm were found to be ranging from 6.32 x 10(-2) to 2.79 x 10(-1)molE(-1) at pH 7. The second-order rate constants of the reaction between the PhACs and OH were determined to be from 4.86 x 10(9) to 6.67 x 10(9)M(-1)s(-1) by using a competition kinetic model which utilized para-chlorobenzoic acid (pCBA) as a reference compound. The overall effect of OH radical scavenging from humic acid (HA) and anions HCO(3)(-), NO(3)(-) was measured utilizing R(OH,UV) method through examining the aqueous photodegradation of pCBA as a probe compound. Moreover, these fundamental direct and indirect photolysis parameters were applied in the model prediction for oxidation rate constants of the PhACs in UV/H(2)O(2) process. It was found that the predicted oxidation rate constants approximated the observed ones. The results indicated that the new R(OH,UV) probe compound method was applicable for measuring background OH radical scavenging effects in water treatment process of UV/H(2)O(2). Furthermore, by GC-MS analysis, most of the intermediates created during the photodegradation of the selected PhACs in UV/H(2)O(2) process were identified. For the photodegradation of PZ, a competition mechanism existed between the direct UV photolysis and the oxidation of OH. An appropriate dosage of H(2)O(2) could hinder the occurrence of the direct photolysis.


Assuntos
Antipirina/análise , Difenidramina/análise , Ibuprofeno/análise , Fenitoína/análise , Biodegradação Ambiental , Peróxido de Hidrogênio , Cinética , Oxirredução , Resíduos de Praguicidas/análise , Fotoquímica/métodos , Fotólise , Espectrofotometria Ultravioleta , Poluentes Químicos da Água/análise
13.
Am J Forensic Med Pathol ; 30(4): 380-1, 2009 Dec.
Artigo em Inglês | MEDLINE | ID: mdl-19901814

RESUMO

Diphenhydramine is a drug readily available over the counter in the form of capsules, tablets, and syrup used for allergy relief. A topical form is sold as a cream without a prescription to alleviate itching. Diphenhydramine is a drug commonly found in postmortem toxicology reports. In rare instances, death is attributed to ingestion of lethal concentrations of the drug. Herein is a report of a toddler who died of lethal concentrations of diphenhydramine from topical application.


Assuntos
Difenidramina/administração & dosagem , Difenidramina/intoxicação , Antagonistas dos Receptores Histamínicos H1/administração & dosagem , Antagonistas dos Receptores Histamínicos H1/intoxicação , Administração Tópica , Edema Encefálico/patologia , Difenidramina/análise , Eczema/tratamento farmacológico , Patologia Legal , Toxicologia Forense , Hemorragia/patologia , Antagonistas dos Receptores Histamínicos H1/análise , Humanos , Lactente , Fígado/química , Pulmão/patologia , Masculino , Miocárdio/patologia , Edema Pulmonar/patologia , Timo/patologia
14.
Sci Total Environ ; 648: 1257-1262, 2019 Jan 15.
Artigo em Inglês | MEDLINE | ID: mdl-30340271

RESUMO

Aquatic systems receive a wide range of pharmaceuticals that may have adverse impacts on aquatic wildlife. Among these pharmaceuticals, antihistamines are commonly found, and these substances have the potential to influence the physiology of aquatic invertebrates. Previous studies have focused on how antihistamines may affect behaviours of aquatic invertebrates, but these studies probably do not capture the full consequences of antihistamine exposure, as traditional recording techniques do not capture important animal movements occurring at the scale of milliseconds, such as prey escape responses. In this study, we investigated if antihistamine exposure can impact escape responses in aquatic insect, by exposing damselfly (Coenagrion hastulatum) larvae to two environmentally relevant concentrations (0.1 and 1 µg L-1) of diphenhydramine. Importantly, we used a high-speed imaging approach that with high-time resolution captures details of escape responses and, thus, potential impacts of diphenhydramine on these behaviours. Our results show overall weak effects of antihistamine exposure on the escape behaviours of damselfly larvae. However, at stage 2 of the C-escape response, we found a significant increase in turning angle, which corresponds to a reduced swimming velocity, indicating a reduced success at evading a predator attack. Thus, we show that low concentrations of an antihistamine may affect behaviours strongly related to fitness of aquatic insect prey - effects that would have been overlooked using traditional recording techniques. Hence, to understand the full consequences of pharmaceutical contamination on aquatic wildlife, high-speed imaging should be incorporated into future environmental risk assessments.


Assuntos
Difenidramina/análise , Reação de Fuga/efeitos dos fármacos , Antagonistas dos Receptores Histamínicos H1/análise , Odonatos/efeitos dos fármacos , Poluentes Químicos da Água/efeitos adversos , Animais , Relação Dose-Resposta a Droga , Larva/efeitos dos fármacos , Odonatos/crescimento & desenvolvimento , Distribuição Aleatória
15.
Artigo em Inglês | MEDLINE | ID: mdl-18926779

RESUMO

Biological matrix effects are a source of significant errors in both electrospray (ESI) and atmospheric pressure chemical ionization (APCI) LC/MS. Glycerophosphocholines (GPChos) and 2-lyso-glycerophosphocholines (2-lyso GPChos) are known to fragment to form ions at m/z 184 and m/z 104, respectively. Phospholipids were used as markers to evaluate matrix effects resulting in both ion suppression and enhancement using ESI and APCI modes in the determination of chlorpheniramine in human plasma. Results revealed that GPChos and 2-lyso GPChos demonstrated very low ionization efficiency in the APCI mode, post-column infusion experiments were performed to confirm that suppression and enhancement matrix ionization effects coincided with the elution profiles of the phospholipids. The mean matrix effect for chlorpheniramine using APCI was 75% less than the mean matrix effect in ESI, making APCI the ionization method of choice initially even though the absolute response was lower than in the ESI mode. The resulting APCI method showed acceptable results according to the FDA guidelines; however, a multiple source relative matrix effects study demonstrated variability. It was concluded that an absolute matrix effects study in one source of biological fluid may be not sufficient to ensure the validity of the method in various sources of matrix. In order to obviate the multiple matrix source variability, we employed an isotopically labeled internal standard for quantification of chlorpheniramine in the ESI mode. An additional validation was completed with the use of chlorpheniramine-d(6) as the internal standard. This method met all acceptance criteria according to the FDA guidelines, and the relative matrix affects study was successful.


Assuntos
Clorfeniramina/sangue , Glicerilfosforilcolina/análise , Lisofosfolipídeos/análise , Espectrometria de Massas por Ionização por Electrospray , Espectrometria de Massas em Tandem , Cromatografia Líquida/métodos , Difenidramina/análise , Glicerilfosforilcolina/química , Antagonistas dos Receptores Histamínicos H1/sangue , Humanos , Lisofosfolipídeos/química , Padrões de Referência , Reprodutibilidade dos Testes , Sensibilidade e Especificidade , Espectrometria de Massas por Ionização por Electrospray/instrumentação , Espectrometria de Massas por Ionização por Electrospray/métodos , Espectrometria de Massas em Tandem/instrumentação , Espectrometria de Massas em Tandem/métodos
16.
Anal Sci ; 24(4): 535-8, 2008 Apr.
Artigo em Inglês | MEDLINE | ID: mdl-18403849

RESUMO

On the basis of the structural interactions between diphenhydramine (DPH) and ephedrine (EPH) to enhance electrochemiluminescence (ECL) intensity, a flow-injection ECL analysis of DPH in the present of EPH by utilizing tris(2,2'-bipyridine)ruthenium(II), (Ru(bpy)(3)2+) has been reported. In the optimized experimental conditions, the linear ECL response to concentrations of DPH is from 2.00 to 40.0 microg/L with a correlation coefficient of 0.9995 and a detection limit of 1.20 microg/L. The relative standard deviation (RSD) was less than 4.6% (n=5) and the recovery was in the range of 98-106% for the determination of DPH in pharmaceutical samples. The method avoids any interference of coexistent EPH in the compounding drug without prior separation. The method has advantages over HPLC method in terms of speed and convenience, economics and safe procedure, and could be an alternative for places where HPLC equipment is not available.


Assuntos
Difenidramina/análise , Efedrina/análise , Cromatografia Líquida de Alta Pressão , Análise de Injeção de Fluxo , Concentração de Íons de Hidrogênio , Medições Luminescentes , Compostos Organometálicos
17.
Artigo em Inglês | MEDLINE | ID: mdl-17553739

RESUMO

Two rapid, simple and sensitive extractive specrophotometric methods has been developed for the determination of three histamine H1-antagonists drugs, e.g., chlorphenoxamine hydrochloride (CPX), diphenhydramine hydrochloride (DPH) and clemastine (CMT) in bulk and in their pharmaceutical formulations. The first method depend upon the reaction of molybdenum(V) thiocyanate ions (Method A) with the cited drugs to form stable ion-pair complexes which extractable with methylene chloride, the orange red color complex was determined colorimetrically at lambda(max) 470nm. The second method is based on the formation of an ion-association complex with alizarin red S as chromogenic reagents in acidic medium (Method B), which is extracted into chloroform. The complexes have a maximum absorbance at 425 and 426nm for (DPH or CMT) and CPX, respectively. Regression analysis of Beer-Lambert plots showed a good correlation in the concentration ranges of 5.0-40 and 5-70microgmL(-1) for molybdenum(V) thiocyanate (Method A) and alizarin red S (Method B), respectively. For more accurate analysis, Ringbom optimum concentration ranges were calculated. The molar absorptivity, Sandell sensitivity, detection and quantification limits were calculated. Applications of the procedure to the analysis of various pharmaceutical preparations gave reproducible and accurate results. Further, the validity of the procedure was confirmed by applying the standard addition technique and the results obtained in good agreement well with those obtained by the official method.


Assuntos
Antagonistas dos Receptores Histamínicos H1/análise , Preparações Farmacêuticas/química , Antraquinonas/química , Clemastina/análise , Clemastina/química , Clemastina/isolamento & purificação , Difenidramina/análise , Difenidramina/química , Difenidramina/isolamento & purificação , Formas de Dosagem , Etilaminas/análise , Etilaminas/química , Etilaminas/isolamento & purificação , Antagonistas dos Receptores Histamínicos H1/química , Antagonistas dos Receptores Histamínicos H1/isolamento & purificação , Concentração de Íons de Hidrogênio , Cinética , Reprodutibilidade dos Testes , Solventes/química , Espectrofotometria , Temperatura , Fatores de Tempo
18.
Forensic Sci Int ; 288: 23-28, 2018 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-29705586

RESUMO

Sleeping aids are often abused in the commission of drug-facilitated crimes. Generally, there is little evidence that a victim ingested a spiked drink unknowingly because the unconscious victim cannot report the situation to the police immediately after the crime occurred. Although conventional segmental hair analysis can estimate the number of months since a targeted drug was ingested, this analysis cannot determine the specific day of ingestion. We recently developed a method of micro-segmental hair analysis using internal temporal markers (ITMs) to estimate the day of drug ingestion. This method was based on volunteer ingestion of ITMs to determine a timescale within individual hair strands, by segmenting a single hair strand at 0.4-mm intervals, corresponding to daily hair growth. This study assessed the ability of this method to estimate the day of ingestion of an over-the-counter sleeping aid, diphenhydramine, which can be easily abused. To model ingestion of a diphenhydramine-spiked drink unknowingly, each subject ingested a dose of diphenhydramine, followed by ingestion of two doses of the ITM, chlorpheniramine, 14days apart. Several hair strands were collected from each subject's scalp several weeks after the second ITM ingestion. Diphenhydramine and ITM were detected at specific regions within individual hair strands. The day of diphenhydramine ingestion was estimated from the distances between the regions and the days of ITM ingestion. The error between estimated and actual ingestion day ranged from -0.1 to 1.9days regardless of subjects and hair collection times. The total time required for micro-segmental analysis of 96 hair segments (hair length: 3.84cm) was approximately 2days and the cost was almost the same as in general drug analysis. This procedure may be applicable to the investigation of crimes facilitated by various drugs.


Assuntos
Crime , Difenidramina/análise , Medicina Legal/métodos , Cabelo/química , Medicamentos Indutores do Sono/análise , Detecção do Abuso de Substâncias/métodos , Bebidas , Biomarcadores/análise , Clorfeniramina/análise , Efedrina/análogos & derivados , Efedrina/análise , Feminino , Humanos , Masculino , Reprodutibilidade dos Testes , Fatores de Tempo
19.
Mar Pollut Bull ; 135: 648-653, 2018 Oct.
Artigo em Inglês | MEDLINE | ID: mdl-30301084

RESUMO

Despite the amount of treated wastewater discharged into the Southern California Bight, few studies have examined pharmaceutical compounds in local biota. The Round Stingray (Urobatis halleri) was selected as a representative elasmobranch species to perform an exploratory study on environmental pharmaceutical exposure. Archived liver samples of males and females from juvenile to adult size classes from several locations (n = 53) were examined for 18 pharmaceutical and illicit drug compounds using isotope-dilution LC-MS/MS. Very few compounds were detected in stingray livers, with diphenhydramine as the only pharmaceutical above quantitation limits. Only stingrays collected from the urban site (mainland California) had detectable levels of diphenhydramine compared to no detections in reference stingrays (offshore island). Sex and sampling location substantially influenced both detection rate and concentrations. Our results suggest that aspects of species' ecology and physiology should be considered for future studies investigating pharmaceutical exposure in elasmobranchs.


Assuntos
Difenidramina/farmacocinética , Rajidae/metabolismo , Poluentes Químicos da Água/análise , Poluentes Químicos da Água/farmacocinética , Animais , California , Difenidramina/análise , Ecotoxicologia/métodos , Exposição Ambiental/análise , Feminino , Fígado/química , Masculino , Preparações Farmacêuticas/análise , Fatores Sexuais
20.
J Mass Spectrom ; 53(11): 1070-1077, 2018 Nov.
Artigo em Inglês | MEDLINE | ID: mdl-30107051

RESUMO

New applications for gold nanoparticles (AuNPs) in laser desorption ionization mass spectrometry are presented here. This work expands on previous biomolecule studies and introduces carbohydrates, steroids, bile acids, and other small molecules as a focus. Broad trends in ionization are observed, and specifically of interest are new species that have not previously been reported from AuNPs (e.g., [M + Au]+ ). Interesting fragmentation effects have been observed for diphenhydramine, including similarity to electron impact mass spectra and possible radical driven reactions, providing insight into the mechanism of ionization when using AuNPs.


Assuntos
Ouro/química , Nanopartículas Metálicas/química , Espectrometria de Massas por Ionização e Dessorção a Laser Assistida por Matriz/métodos , Ácidos e Sais Biliares/análise , Ácidos e Sais Biliares/química , Carboidratos/análise , Carboidratos/química , Difenidramina/análise , Difenidramina/química , Esteroides/análise , Esteroides/química
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