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The selectivity of a suitable organic solvent is key for extraction in liquid-phase microextraction experiments. Nevertheless, the screening process remains a daunting task. Our research aimed to study the relationship between extraction efficiency and extraction solvents, analytes, and finally select the appropriate extraction solvent. In the present article, ß-blockers and six extraction solvents were chosen as the models and hollow-fiber liquid-phase microextraction was conducted. The relationship was built by statistical analysis on the data. Factors affecting extraction efficiency including the logarithms of the octanol/water partition coefficient (logPo/w ) of analytes, acid dissociation constants, the logarithms of the octanol/water partition coefficient of solvents and pH of the sample solution were investigated. The results showed that a low water solubility of extraction solvent is the foundation to ensure higher extraction efficiency. Moreover, when ΔlogPo/w > 0, a higher extraction efficiency is observed at lower ΔlogPo/w , on the contrary, when ΔlogPo/w < 0, extraction efficiency is higher as the absolute value of ΔlogPo/w becomes greater. Finally, the relationship between enrichment factor and extraction solvents, analytes was established and a helpful guidance was provided for the selection of an optimal solvent to obtain the best extraction efficiency by liquid-phase microextraction.
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Antagonistas Adrenérgicos beta/análise , Microextração em Fase Líquida/métodos , Álcoois Graxos , Humanos , Concentração de Íons de Hidrogênio , Modelos Químicos , SolventesRESUMO
To establish an EDTA complexation extraction pretreatment combining with GFAAS method for the determination of residual aluminium ion in Huoxiang zhengqi pellets without digestive treatment, systematical investigation was made on sample preparation, and EDTA was used for the complexation extraction of residual aluminium ion in samples. The pH, concentration and volume of extraction solution, the temperature and time of microwave extraction, and graphite furnace temperature program were investigated. The results were compared with the microwave digestion. It was showed that, 0.1 g of sample weight was added in 20 mL 0.05 mol x L(-1) EDTA solution (pH 3.5), followed by heating at 150 degrees C for 10 min in the microwave extraction device. The determination of GFAAS was performed at optimized detection wavelength (257.4 nm) as well as graphite furnace temperature program, the detection limits and quantification limits were 2.37 µg x L(-1) and 7.89 µg x L(-1), respectively. The precision (RSD) was less than 2.3%. The average recovery was 96.9% -101%. The present method is easy, rapid and accurate for the determination of residual aluminium ion in Huoxiang zhengqi pellets.
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Alumínio/química , Alumínio/isolamento & purificação , Contaminação de Medicamentos , Medicamentos de Ervas Chinesas/química , Espectrofotometria Atômica/métodos , Ácido Edético/química , Grafite/química , TemperaturaRESUMO
OBJECTIVE: Myocardial contrast echocardiography (MCE) plays a crucial role in diagnosing ischemia, infarction, masses and other cardiac conditions. In the realm of MCE image analysis, accurate and consistent myocardial segmentation results are essential for enabling automated analysis of various heart diseases. However, current manual diagnostic methods in MCE suffer from poor repeatability and limited clinical applicability. MCE images often exhibit low quality and high noise due to the instability of ultrasound signals, while interference structures can further disrupt segmentation consistency. METHODS: To overcome these challenges, we proposed a deep-learning network for the segmentation of MCE. This architecture leverages dilated convolutions to capture high-scale information without sacrificing positional accuracy and modifies multi-head self-attention to enhance global context and ensure consistency, effectively overcoming issues related to low image quality and interference. Furthermore, we also adapted the cascade application of transformers with convolutional neural networks for improved segmentation in MCE. RESULTS: In our experiments, our architecture achieved the best Dice score of 84.35% for standard MCE views compared with that of several state-of-the-art segmentation models. For non-standard views and frames with interfering structures (mass), our models also attained the best Dice scores of 83.33% and 83.97%, respectively. CONCLUSION: These studies proved that our architecture is of excellent shape consistency and robustness, which allows it to deal with segmentation of various types of MCE. Our relatively precise and consistent myocardial segmentation results provide fundamental conditions for the automated analysis of various heart diseases, with the potential to discover underlying pathological features and reduce healthcare costs.
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AIM: People today have a stronger interest in the risk of biosafety in clinical bioanalysis. A safe, simple, effective method of preparation is needed urgently. METHODOLOGY/RESULTS: To improve biosafety of clinical analysis, we used antiviral drugs of adefovir and tenofovir as model drugs and developed a safe pretreatment method combining sealing technique with direct injection technique. The inter- and intraday precision (RSD %) of the method were <4%, and the extraction recoveries ranged from 99.4 to 100.7%. Meanwhile, the results showed that standard solution could be used to prepare calibration curve instead of spiking plasma, acquiring more accuracy result. CONCLUSION/DISCUSSION: Compared with traditional methods, the novel method not only improved biosecurity of the pretreatment method significantly, but also achieved several advantages including higher precision, favorable sensitivity and satisfactory recovery. With these highly practical and desirable characteristics, the novel method may become a feasible platform in bioanalysis.
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Adenina/análogos & derivados , Antivirais/sangue , Técnicas de Laboratório Clínico/métodos , Organofosfonatos/sangue , Tenofovir/sangue , Adenina/sangue , Adenina/isolamento & purificação , Antivirais/isolamento & purificação , Cromatografia Líquida de Alta Pressão , Técnicas de Laboratório Clínico/instrumentação , Técnicas de Laboratório Clínico/normas , Humanos , Limite de Detecção , Organofosfonatos/isolamento & purificação , Tenofovir/isolamento & purificação , Ultrafiltração/instrumentação , Viroses/prevenção & controleRESUMO
AIM: Plasma protein binding (PPB), as a significant influenced factor of pharmacokinetic and pharmacodynamic properties of a medicine, is a suitable index for therapeutic drug monitoring (TDM) strategies. A suitable measurement technique of PPB of patients is in urgent need and attracts many analysts' attention. Results & methodology: In this study, a novel method was proposed to analyze free drug concentration and total drug concentration (Ct) successively in one unit with a sample. All RSDs were less than 3%. The absolute recovery of Ct ranged from 98.1 to 101.2%. DISCUSSION & CONCLUSION: It is extremely valuable to consider PPB as an important index for TDM, perfecting information of medication, reflecting the disease condition more comprehensively, providing assistance for doctors to adjust the dose regimen. The proposed technique, convenience, accuracy and without the influence of plasma condition, provides a feasible method to monitor PPB of various patients, facilitating the popularization of monitoring PPB in TDM.
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Aminofilina/metabolismo , Proteínas Sanguíneas/metabolismo , Centrifugação/métodos , Monitoramento de Medicamentos/métodos , Plasma/metabolismo , Doenças Respiratórias/tratamento farmacológico , Ultrafiltração/métodos , Adulto , Idoso , Idoso de 80 Anos ou mais , Broncodilatadores/metabolismo , Feminino , Humanos , Masculino , Pessoa de Meia-Idade , Ligação Proteica , Doenças Respiratórias/metabolismo , Ultrafiltração/instrumentaçãoRESUMO
To examine how methods affect the evaluation of entrapment efficiency (EE) of liposomes, four different sample pretreatment methods were adopted in the experiment. The four sample pretreatment methods were size-exclusion chromatography (SEC), solid-phase extraction (SPE), centrifugation ultrafiltration (CF-UF) and hollow fiber centrifugal ultrafiltration (HF-CF-UF). Amphotericin B (AmB), which could self-associate to form aggregates in water is adopted as the model drugs in this paper. In the present work, it was found that the characterization results of four methods were quite different. The EE of liposome by SEC was about 93%, only 5-13% using C18 or HLB columns, and approximately 100% by CF-UF. The EE of HF-CF-UF reached up to nearly 99.0%. Further, this paper revealed the reasons making the difference of EE among four methods. Conventional SEC may distort the authentic of EE of liposomes with mainly employing some small liposomes or excessive water as eluent. For SPE, cholesterol on liposome surface could interact with the stationary phase making it hard to elute with water, and increase the risk of liposome leakage. While for CF-UF, concentration polarization was a main limitation hindering unentrapped drug to pass through membrane, making unentrapped drug undetectable in liposome. HF-CF-UF could truly reflect EE of liposomes with the concentration of unentrapped AmB lower than 25.0µg/mL. However, when the concentration was higher than 25.0µg/mL, AmB aggregates could be entrapped by hollow fiber. From the above analysis, this paper came to the conclusion that each method had its own feature in characterization. This study provided a reasonable guideline for choosing methods to character the EE of liposome.