RESUMEN
BACKGROUND: There is ongoing debate regarding which embryo transfer procedure can achieve a higher live birth rate. Research has suggested that frozen ET might be beneficial for certain populations, such as hyper-responders. This study aimed to compare outcomes of pregnancies between frozen and fresh embryo transfer cycles in patients with endometrial hyperplasia and carcinoma. METHODS: This retrospective cohort study was conducted at a high-volume reproductive center from January 2010 to January 2022. Patients who were diagnosed with endometrial hyperplasia with atypia and endometrial carcinoma were included. They all underwent in vitro fertilization after conservative treatment. The primary outcome was live birth after frozen and fresh embryo transfer cycles, and secondary outcomes included perinatal complications and other pregnancy outcomes. RESULTS: Overall, 259 ET cycles (130 fresh and 129 frozen) were included. The rate of live births per embryo transfer cycle of the whole cohort was 20.8% (54/259), and no significant between-group difference was found after adjusting for potential confounding factors (23.8% vs. 17.8%; adjusted OR, 0.47; 95% CI, 0.21-1.06; p=0.068). Compared to fresh embryo transfer group, the incidence of total maternal complications in the frozen embryo transfer group was significantly higher (30.4% vs. 6.5%, p=0.019). Analyzing each complication as a separate entity, patients in the frozen embryo transfer group had a higher incidence of hypertensive disorders of pregnancy (p=0.028). Multiple logistic regression analysis showed that frozen embryo transfer was related with an increased occurrence of maternal complications (OR, 6.68, 95% CI, 1.01-44.19, p=0.040). CONCLUSIONS: Among patients with endometrial hyperplasia and carcinoma, the rate of live births was comparable between both embryo transfer procedures, while frozen embryo transfer might be associated with a higher risk of maternal complications compared to that with fresh embryo transfer.
Asunto(s)
Carcinoma , Hiperplasia Endometrial , Embarazo , Femenino , Humanos , Estudios Retrospectivos , Hiperplasia Endometrial/epidemiología , Criopreservación/métodos , Transferencia de Embrión/métodos , Fertilización In Vitro/métodos , Nacimiento Vivo/epidemiología , Índice de EmbarazoRESUMEN
PURPOSE: To investigate the in vitro fertilization/intracytoplasmic sperm injection (IVF/ICSI) outcomes and identify factors that might affect live births in patients with early-stage endometrial cancer (EEC) and atypical endometrial hyperplasia (AEH). METHODS: This retrospective study was performed in a tertiary hospital. Patients (n = 123) with EEC or AEH, who underwent IVF/ICSI treatment between January 2010 and December 2019, were divided into a live birth group and a non-live birth group. Clinical characteristics and IVF/ICSI outcomes were assessed. RESULTS: A total of 123 patients (28 with EEC and 95 with AEH) underwent 215 ovarian stimulation cycles, resulting in 121 fresh embryo transfer (ET) and 108 frozen-thawed ET. Among 229 ET cycles, 91 (23.7%) of 384 embryos were implanted and 86 pregnancies were achieved, including five ectopic pregnancies (5.8%), 28 miscarriages (32.6%), and 53 live births (61.6%). The clinical pregnancy and live birth rates in each ET cycle were 37.6% and 23.1%, respectively. Fifty-one patients gave birth to 57 live neonates, and the cumulative live birth rate was 41.46%. Multiple logistic regression analysis showed that maternal age, histological type, thin endometrium, and time after complete remission (CR) to IVF cycle started were significantly associated with live births. CONCLUSIONS: The live birth rate after IVF/ICSI is promising in infertile patients with EEC and AEH. A shorter interval between CR and IVF/ICSI treatment might be a positive factor, while age > 35 years, endometrial thickness < 8 mm on the day of ET, and degree of endometrial lesion progressing into carcinoma can negatively influence IVF/ICSI outcomes.
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Hiperplasia Endometrial , Neoplasias Endometriales , Infertilidad Femenina , Adulto , Tasa de Natalidad , Tratamiento Conservador , Hiperplasia Endometrial/complicaciones , Neoplasias Endometriales/complicaciones , Endometrio , Femenino , Fertilización In Vitro/métodos , Humanos , Recién Nacido , Infertilidad Femenina/terapia , Masculino , Embarazo , Índice de Embarazo , Estudios Retrospectivos , Semen , Inyecciones de Esperma Intracitoplasmáticas/métodosRESUMEN
Nuclear receptor coactivator 5 (NCOA5) specifically enhances estrogen receptor α-modulated transcriptional activity. As a novel tumor suppressor, depletion of NCOA5 is associated with the development of a variety of tumors, but its function in cervical cancer is currently unclear. In this study, we addressed how expression of NCOA5 changed in the development of human cervical cancer and its association with clinicopathological features, prognosis, and biology characteristics of cervical cancer. Analysis of the microarrays in the Oncomine database indicated that NCOA5 expression was lower in human cervical squamous cell carcinoma tissues than that in normal cervical tissues. That was corroborated by our experiments using fresh tissues: the expression levels of NCOA5 messenger RNA and protein were both significantly decreased in cervical cancer tissues compared with paired adjacent nontumor tissues (P < 0.01). Low expression of NCOA5 is associated with the International Federation of Gynecology and Obstetrics stage ( P = 0.043) and histological grade ( P = 0.018) of human cervical cancer. In addition, patients possessing low NCOA5 expression had poorer prognosis. Univariate and multivariate Cox regression analyses indicated that low NCOA5 expression may be an independent prognostic factor for poorer overall survival in cervical cancer. Further, downregulation of NCOA5 expression results in a significant increase in proliferation, migration, and invasion of HeLa cells. Data of xenograft tumor on BALB/c nude mice manifested that HeLa cells with low NCOA5 expression tend to form larger tumors than negative control ones. In contrast, overexpression of NCOA5 expression leads to the opposite results. Finally, we found that NCOA5 might affect the biological function of human cervical cancer cells by mediating the notch3 signaling pathway. These findings suggest that NCOA5 acts as a tumor suppressor to inhibit tumorigenicity, migration, and invasion, and thus represents a potential novel prognostic marker for overall survival in cervical cancer.
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Regulación hacia Abajo , Coactivadores de Receptor Nuclear/genética , Coactivadores de Receptor Nuclear/metabolismo , Transducción de Señal , Neoplasias del Cuello Uterino/patología , Adulto , Animales , Línea Celular Tumoral , Movimiento Celular , Proliferación Celular , Femenino , Regulación Neoplásica de la Expresión Génica , Células HeLa , Humanos , Ratones , Persona de Mediana Edad , Clasificación del Tumor , Invasividad Neoplásica , Trasplante de Neoplasias , Pronóstico , Receptor Notch3/metabolismo , Análisis de Supervivencia , Neoplasias del Cuello Uterino/genética , Neoplasias del Cuello Uterino/metabolismoRESUMEN
Porous electron-rich organic frameworks have attracted an increased attention in the adsorption and removal of pollutants due to their abundant electron-rich nitrogen atoms, which can effectively interact with positively charged substance. In this study, a porous electron-rich organic framework (Car-POF) and positively charged amino-functionalized magnetic nanoparticles (Fe3O4-NH2) were used to construct a magnetic electron-rich Fe3O4-NH2@Car-POF for the enrichment of some phenylurea herbicides from water and milk samples prior to high performance liquid chromatographic detection. The adsorption capacity of Fe3O4-NH2@Car-POF for the phenylureas ranged from 14.93 to 28.83 mg g-1. The LODs were observed in the range of 0.05-0.20 ng mL-1 and 0.5-1.5 ng mL-1, and LOQs in the range of 0.17-0.66 ng mL-1 and 1.7-5.0 ng mL-1 for water and milk samples with RSD less than 9.0. The adsorption studies with cationic and anionic dyes revealed that Fe3O4-NH2@Car-POF is favorable for the adsorption of positively charged compounds.
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Herbicidas , Estructuras Metalorgánicas , Leche , Compuestos de Fenilurea , Contaminantes Químicos del Agua , Leche/química , Cromatografía Líquida de Alta Presión , Herbicidas/química , Herbicidas/aislamiento & purificación , Animales , Adsorción , Estructuras Metalorgánicas/química , Contaminantes Químicos del Agua/química , Contaminantes Químicos del Agua/aislamiento & purificación , Compuestos de Fenilurea/química , Compuestos de Fenilurea/aislamiento & purificación , Compuestos de Fenilurea/análisis , Porosidad , Nanopartículas de Magnetita/química , Contaminación de Alimentos/análisis , ElectronesRESUMEN
Two magnetic phosphazene-based hyper crosslinked polymers (M-HCP-OP-TMC and M-HCP-OP-TCL) were newly synthesized by the reaction of Friedel-Crafts acylation, and the M-HCP-OP-TMC showed an excellent extraction capability and rapid adsorption kinetics for chlorophenols as an adsorbent. Then, an efficient analytical method was built for the preconcentration and quantification of chlorophenols from water and peach juice samples by combining M-HCP-OP-TMC based magnetic solid-phase extraction (MSPE) with HPLC-UV detection. The linear response range for the chlorophenols by the method was 0.21-100.0 ng mL-1 for water sample, and 0.36-100.0 ng mL-1 for peach juice sample. The detection limits (S/N = 3) of the proposed method for the analytes were 0.07- 0.25 ng mL-1 and 0.12-0.45 ng mL-1 for water and peach juice samples, respectively. The method recoveries for the spiked samples were in the range of 93.1%-117.1%, and the relative standard deviations were less than 10%. The adsorption of the chlorophenols with the M-HCP-OP-TMC was mainly contributed by π-π stacking and hydrophobic interactions. The results indicate that the method was sensitive and accurate enough for the determination of the chlorophenols from real samples.
Asunto(s)
Clorofenoles , Prunus persica , Agua/química , Clorofenoles/análisis , Polímeros/química , Cromatografía Líquida de Alta Presión/métodos , Extracción en Fase Sólida/métodos , Adsorción , Fenómenos Magnéticos , Límite de DetecciónRESUMEN
Developing novel nanoscale carriers for drug delivery is of great significance for improving treatment efficiency and reducing side effects of antitumor drugs. In view of the good biocompatibility and special affinity of porphyrin (PP) molecule to cancer cells, it was used to construct a series of metal-doped M@PP (M = Ca â¼ Zn) materials for the delivery of anticancer drug 5-fluorouracil (5-Fu) in this work. Our results reveal that 5-Fu is tightly adsorbed on M@PP (M = Ca â¼ V, Mn â¼ Co, and Zn) by chemisorption, but is physically adsorbed by M@PP (M = Cr, Ni, and Cu). The calculated electronic properties show that all these 5-Fu@[M@PP] (M = Ca â¼ Zn) complexes have both high stability and solubility. Among these 5-Fu@[M@PP] complexes, the chemical bond formed between 5-Fu and Ti@PP has the strongest covalent characteristic, resulting in the largest adsorption energy of -19.93 kcal/mol for 5-Fu@[Ti@PP]. In particular, 5-Fu@[Ti@PP] has the proper recovery time under the near-infrared light at body temperature, which further suggests that Ti@PP is the best drug carrier for 5-Fu. This study not only reveals the interaction strength and nature between 5-Fu and M@PP, but also confirmed the intriguing potential of Ti@PP as nano-carrier for drug delivery. However, further experimental research should be conducted to verify the conclusion obtained in this work.
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Antineoplásicos , Metaloporfirinas , Portadores de Fármacos , Fluorouracilo/farmacología , Sistemas de Liberación de MedicamentosRESUMEN
A new carbazole-based spherical microporous polymer (Car-BDA-POP) was fabricated by employing 4,4'-biphenyldicarboxaldehyde (BDA) and carbazole as monomers via a one-step and non-metal catalyst synthetic approach. It was then explored as an adsorbent for solid-phase extraction (SPE) of some chlorophenols (CPs). Under the optimized extraction conditions, the established Car-BDA-POP-based SPE coupled with high-performance liquid chromatography ultraviolet detection showed good linearity in the concentration range of 0.1-200 ng mL-1 for water samples and 5.0-800 ng g-1 for honey samples with the determination coefficients (r2) ≥ 0.9995 for the analytes. The limits of detection (S/N = 3) for the analytes were in the range of 0.03-0.06 ng mL-1 for water samples and 1.50-2.50 ng g-1 for honey samples. The method recoveries varied from 80.0 % to 116 % in spiked real samples, with the relative standard deviations less than 9.6 %. In addition, the possible adsorption mechanism, adsorption kinetics, and adsorption isotherms were also investigated.
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Clorofenoles , Miel , Carbazoles/análisis , Clorofenoles/análisis , Cromatografía Líquida de Alta Presión/métodos , Miel/análisis , Polímeros/química , Extracción en Fase Sólida/métodos , AguaRESUMEN
In this work, a series of 5,10,15,20-tetraphenylporphyrin (TPP)-based hyper crosslinked polymers were prepared by Friedel-Crafts reaction. Among them, the HCP-TPP-BCMBP, which was prepared by using TPP as the monomer and with 4,4'-Bis(chloromethyl)-1,1'-biphenyl (BCMBP) as the cross-linking agent, had the best adsorption capability for the enrichment of the nitroimidazoles of dimetridazole, ronidazole, secnidazole, metronidazole, and ornidazole. Then, a solid-phase extraction (SPE) method with the HCP-TPP-BCMBP as adsorbent coupled with HPLC-UV detection for the determination of nitroimidazole residues in honey, environmental water, and chicken breast samples was established. The influence of the main factors that affect the SPE, i.e., sample solution volume, sample loading rate, sample pH, and eluent and its volume, were studied. Under the optimal conditions, the limits of detection (S/N = 3) for the nitroimidazoles were measured to be in the range of 0.02-0.04 ng mL-1, 0.4-1.0 ng g-1 and 0.5-0.7 ng g-1 for environmental water, honey, and chicken breast samples, with the determination coefficients being in the range of 0.9933-0.9998. The analytes recoveries by the method in fortified samples fell in the range from 91.1% to 102.7% for environmental water, from 83.2% to 105.0% for honey, and from 85.9% to 103.0% for chicken breast samples, and the relative standard deviations for the determination were less than 10%. It shows that the HCP-TPP-BCMBP has a strong adsorption capability for some polar compounds.
Asunto(s)
Miel , Nitroimidazoles , Animales , Nitroimidazoles/análisis , Pollos , Agua , Miel/análisis , Polímeros/química , Cromatografía Líquida de Alta Presión/métodos , Extracción en Fase Sólida/métodos , Límite de DetecciónRESUMEN
Purpose: To explore the relationship between different artificial reproductive treatment (ART) strategies and tumor outcomes, by analyzing clinical data of patients with endometrial carcinoma (EC) and atypical endometrial hyperplasia (AEH). Methods: This retrospective study was performed in a tertiary hospital. Patients (n=131) with EC or AEH, who underwent in vitro fertilization (IVF)/intracytoplasmic sperm injection (ICSI) treatment between June 2010 and June 2021, were divided into a recurrence group and a non-recurrence group. Clinical characteristics and tumor outcomes were assessed. Results: 131 patients were followed up for 4-132 months; 33 patients had recurrence, the recurrence rate was 25.2%, 3-year recurrence-free survival (RFS) rate was 83.2 ± 3.4%, and the 5-year RFS rate was 72.9 ± 4.4%. Factors including the frequency of controlled ovarian stimulation (COS) and the total days of ovarian stimulation had no significant effect on the recurrence of tumor lesions (p=0.368 and 0.969, respectively). Histology type (HR: 4.94, 95%CI: 2.41-10.15, p <0.001) and successful/un successful live birth (HR: 0.30, 95%CI: 0.14-0.65, p=0.003) were independent factors of recurrence. Twenty-two of the 82 patients who received a single COS had recurrence. Different COS protocols, the total dose of gonadotropin (Gn), and the serum E2 level on the trigger day had no significant effect on recurrence (p=0.326, 0.889 and 0.468, respectively). Conclusions: The degree at which an endometrial lesion progresses into carcinoma is a key factor affecting the recurrence of EC/AEH in patients after IVF/ICSI treatment, and successful live birth is a protective factor for the recurrence of endometrial lesions. Different COS protocols and COS frequencies, as well as the dosage and duration of Gn used during IVF did not affect the recurrence of endometrial lesions.
RESUMEN
Three magnetic covalent organic frameworks (named M-TpPa-SO3Na, M-TpPa-SO3H and M-TpPa) were prepared by the solvothermal synthesis method with 1,3,5-trimethylphenol (TP) and either 2-sulfo-1,4-phenylenediamine (Pa-SO3H) or p-phenylenediamine (Pa) as monomers. Among them, the M-TpPa-SO3Na possessed relatively high hydrophilicity, good magnetic responsiveness, and high affinity for the benzoylureas (BUs) insecticides. It was then explored as the magnetic solid-phase extraction adsorbent for the extraction of six BUs (diflubenzuron, triflumuron, hexaflumuron, teflubenzuron, flufenoxuron and chlorfluazuron) from water, pear juice and honey samples prior to high-performance liquid chromatography with ultraviolet detection. Under the optimized experimental conditions, a good linearity was achieved within the concentration range of 0.27-40.0 ng mL-1 for water sample, 0.47-30.0 ng mL-1 for pear juice sample, and 2.70-200.0 ng g-1 for honey sample. The limits of detection for the analytes were 0.08-0.11 ng mL-1 for water sample, 0.14-0.19 ng mL-1 for pear juice sample and 0.80-1.00 ng g-1 for honey sample. The method recoveries for spiked samples were in the range of 85.0%-111.0% with the relative standard deviations less than 8.8%. The developed method was successfully used for the determination of the BUs in water, pear juice and honey samples.
Asunto(s)
Miel , Insecticidas , Estructuras Metalorgánicas , Pyrus , Cromatografía Líquida de Alta Presión , Límite de Detección , Fenómenos Magnéticos , Extracción en Fase Sólida , AguaRESUMEN
As plant regulators, auxins can promote plant growth. However, they have toxicity and may cause harm to humans. Due to their low concentrations in food sample matrices, the enrichment and analysis of trace auxins in food samples is a challenging work. In this work, a series of hyper crosslinked polymers (HCPs) were synthesized by Friedel-Crafts acylation to extract four auxins (indole-3-acetic acid, indole-3-propionic acid, indole-3-butyric acid and 1-naphthylacetic acid). Among these HCPs, the QP-TC-HCP, synthesized from p-quaterphenyl (QP) and terephthaloyl chloride (TC), showed the best adsorption performance for the auxins. It was then applied as the adsorbent for the solid-phase extraction of the auxins from environmental water and peach beverage samples, followed by high performance liquid chromatography-fluorescence detection. Under the optimized conditions, the limits of detection were 3.0-12.0 pg mL-1 for environmental water and 18.0-36.0 pg mL-1 for peach beverage sample. The method recoveries of the auxins for the spiked samples were in the range of 85.0-110.0%. The established method provided an alternative approach for the determination of auxins in food samples. In addition, different types of organic compounds were tested for the extraction by the QP-TC-HCP to assess its application potential and adsorption mechanism. It was concluded that the QP-TC-HCP had better extraction performance for the compounds with certain hydrophilicity and more hydrogen bonding sites.
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Polímeros , Prunus persica , Adsorción , Bebidas/análisis , Cromatografía Líquida de Alta Presión/métodos , Humanos , Ácidos Indolacéticos/análisis , Límite de Detección , Polímeros/análisis , Extracción en Fase Sólida/métodos , AguaRESUMEN
The three hypercrosslinked polymers (HCP) materials, designated as OPD-HCP, MPD-HCP and PPD-HCP, were synthesized by using o-phenylenediamine (OPD), m-phenylenediamine (MPD) and p-phenylenediamine (PPD) as monomers. They were characterized by infrared spectroscopy, powder X-ray diffraction, nitrogen sorption isotherms, and scanning electron microscopy. Then, the HCPs were explored as solid-phase extraction (SPE) adsorbent for the extraction of five nitroimidazoles (NDZs) (metronidazole, ronidazole, secnidazole, dimetridazole and ornidazole). Among the three HCPs, the MPD-HCP has the best adsorption performance for the NDZs. With the help of high-performance liquid chromatography with ultraviolet detection (HPLC-UV), good linear response range (0.07-40.0 ng mL-1), high method recovery (86.8%-113.3%), low limits of detection (0.02-0.15 ng mL-1) and good precision with the relative standard deviations of less than 8.1% were achieved for the determination of the NDZs in water samples. The effective determination of the NDZs in peach juice, honey tea, and honey samples were also realized by the developed method with satisfactory results. Based on both the experimental results and density functional theory calculation, the adsorption mechanism can be attributed to multiple interactions between the MPD-HCP and the NDZs, including hydrogen bonding, hydrophilic, and electrostatic interactions. The method provides a new alternative of choice for the determination of some NDZs in real samples.
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Miel , Nitroimidazoles , Cromatografía Líquida de Alta Presión/métodos , Miel/análisis , Límite de Detección , Nitroimidazoles/análisis , Polímeros/química , Extracción en Fase Sólida/métodos , Agua/químicaRESUMEN
In this work, a porous extended network covalent organic framework designated as TP-NDA-COF was synthesized by the reaction of 2,4,6-trihydroxy-benzene-1,3,5-tricarbaldehyde (TP) and 1,5-naphthalenediamine (NDA). The structure and morphology of the TP-NDA-COF was characterized by means of Fourier transform infrared spectra (FT-IR), thermal gravimetric analysis (TGA), X-ray diffraction (XRD) and scanning electron microscope (SEM). The TP-NDA-COF was applied as a solid-phase extraction adsorbent for the extraction of some chlorophenols from water and lemon black tea beverage samples prior to high performance liquid chromatography-UV detection. The main experimental parameters that affect the extraction efficiency including the type and volume of eluent, sample solution volume, sample loading rate and sample solution pH were investigated. Under the optimal conditions, the calibration curves were linear in the range of 0.30-60.0 ng mL-1 with the determination coefficients (R2) of 0.9996-0.9998 for water samples and in the range of 0.60-60.0 ng mL-1 with the R2 values from 0.9990 to 0.9996 for beverage samples. At the signal to noise ratio of 3 (S/N = 3), the method LODs for the analytes were 0.10-0.15 ng mL-1 for water samples and 0.20-0.50 ng mL-1 for lemon black tea beverage, respectively. Good repeatability was achieved with the relative standard deviations of less than 7%. The results showed that the SPE-HPLC method can be used for the determination of chlorophenols in environmental water and foodstuffs samples.
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Clorofenoles , Estructuras Metalorgánicas , Adsorción , Clorofenoles/análisis , Cromatografía Líquida de Alta Presión/métodos , Límite de Detección , Estructuras Metalorgánicas/química , Extracción en Fase Sólida/métodos , Espectroscopía Infrarroja por Transformada de Fourier , Té/química , Agua/químicaRESUMEN
A uniform spherical structure covalent organic framework (TAPA-BPDA-COF) was prepared by a facile method at room temperature with tris(4-aminophenyl)amine (TAPA) and 4,4'-biphenyldicarboxaldehyde (BPDA) as building blocks. Based on the solid phase extraction with the TAPA-BPDA-COF as the sorbent and high performance liquid chromatography-diode array detection, a sensitive analytical method was established for the determination of four neonicotinoid insecticides from water and honey samples. Under the optimum conditions, good linear response for the quantification of the analytes was achieved in the range of 0.3-50.0 ng mL-1 for water samples and in the range of 8.0-500.0 ng g-1 for honey samples. The method recoveries fell in the range of 80.0-121.9% with RSDs less than 7.6%. The limits of detection at the signal to noise ratio of 3 were measured to be in the range of 0.08-0.12 ng mL-1 for water samples and 2.6-3.3 ng g-1 for honey samples, depending on compounds.
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Insecticidas , Estructuras Metalorgánicas , Cromatografía Líquida de Alta Presión , Límite de Detección , Neonicotinoides , Extracción en Fase SólidaRESUMEN
In this work, a novel knitting aromatic polymer (KAP) was fabricated for the first time by knitting ferrocene with 1,3,5-tris(bromomethyl)-2,4,6-trimethylbenzene via Friedel-Crafts reaction, and then the KAP was magnetically functionalized with Fe3O4 nanoparticles to produce a magnetic KAP (M-KAP). Combining M-KAP based magnetic solid-phase extraction with high performance liquid chromatography-ultraviolet detection, a simple and sensitive method was developed for simultaneous determination of six benzoylurea insecticides (BUs) in honey and apple juice samples. In the optimized conditions, a good linearity for the BUs existed in the range of 1.67-1000 ng g-1 for honey sample and 0.500-100.0 ng mL-1 for apple juice sample. The limits of detection were 0.500-1.50 ng g-1 and 0.150-0.400 ng mL-1 for honey and apple juice sample, respectively. Satisfactory recoveries were in the range of 85.5-105.5% with RSDs ≤ 8.3%. The developed method demonstrated an excellent practicability for sensitive analysis of the BUs.
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Miel , Insecticidas , Malus , Cromatografía Líquida de Alta Presión/métodos , Miel/análisis , Insecticidas/análisis , Límite de Detección , Fenómenos Magnéticos , Polímeros/análisis , Extracción en Fase Sólida/métodosRESUMEN
A triazine-based porous organic polymer was prepared by facile solvothermal polymerization with cyanuric chloride and triphenyl phosphine as functional monomers. The polymer was characterized and then used for the first time as the sorbent for the effective solid-phase extraction of some nitroimidazoles (NDZs) (metronidazole, ronidazole, secnidazole, dimetridazole and ornidazole). The main experimental influencing parameters for the extraction including the eluent solvent, eluent volume, sample loading rate, sample solution pH, salt concentration and sample volume were investigated. The adsorption kinetics and adsorption isotherms were investigated to elucidate the possible adsorption mechanism. With the triazine-based porous organic polymer as the SPE adsorbent, trace NDZs were effectively extracted. The good enrichment capability for the NDZs was mainly attributed to the hydrogen binding interactions by the aromatic 1,3,5-trizine rings. After the SPE, the extracted analytes were analyzed by high-performance liquid chromatograph with ultraviolet detection. Under the selected conditions, the method had a good linear response for the analytes in the range of 0.06-120 ng mL-1 for water and 1.5-1200 ng g-1 for honey samples. The limits of detections (S/N=3) fell in the range of 0.02-0.06 ng mL-1 for water and 0.5-1.5 ng g-1 for honey samples. The method recoveries for the analytes for spiked samples were in the range of 80.3-118%. The method can be applied for the determination of the NDZs from real samples.
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Miel/análisis , Nitroimidazoles/aislamiento & purificación , Compuestos Organofosforados/química , Polímeros/química , Extracción en Fase Sólida/métodos , Triazinas/química , Contaminantes Químicos del Agua/aislamiento & purificación , Adsorción , Cromatografía Líquida de Alta Presión/métodos , Límite de Detección , Porosidad , Agua/químicaRESUMEN
A carbazolic conjugated microporous polymer (designated as CZ-CMP) was successfully synthesized through Scholl reaction of carbazole with 1, 3, 5-triphenylbenzene. The CZ-CMP was characterized by FT-IR spectrum, X-ray diffraction, nitrogen sorption isotherms, and scanning electron microscopy. The characterization results showed that the CZ-CMP had a spherical structure with high surface area and good microporosity. Its adsorption performance was investigated by applying it as an adsorbent for the solid phase extraction (SPE) of phenyl urea herbicides (PUHs) (metoxuron, chlortoluron, isoproturon, monolinuron and buturon) from tea drinks samples prior to high performance liquid chromatographic detection. The CZ-CMP displayed high extraction efficiency for the PUHs, and the primary factors affecting the SPE efficiency including the type and volume of the eluent, sample solution pH, sample loading rate and sample volume were optimized. Under the optimized conditions, a good linear response for the analytes was observed in the range of 0.10-80.0 ng mL-1 with correlation coefficients (r) from 0.9937 to 0.9997. The limits of detection were measured to be in the range of 0.02-0.30 ng mL-1 and the limits of quantitation were in the range of 0.06-0.9 ng mL-1. The developed method was successfully applied for the determination of the five PUHs in four different kinds of drinks with the method recoveries between 83.7% and 118% and the relative standard deviations between 1.0% and 10%. Besides, the application potential of the CZ-CMP was evaluated by using it to extract different types of the organic compounds including some phthalate eaters (PAEs), chlorophenol (CPs), nitroimidazoles and polycyclic aromatic hydrocarbons (PAHs). The results indicated that the CZ-CMP had strong adsorption ability for the compounds with more hydrogen bonding sites and moderate hydrophobicity.