Determination of Enantiomeric Composition of Substituted Tetrahydroisoquinolines Based on Derivatization with Menthyl Chloroformate

A method for the analysis of the optical purity of a series of chiral substituted tetrahydroisoquinolines (THIQs) was developed. The method is based on pre-column derivatization of the analytes with the derivatization reagent (–)-(1R)-menthyl chloroformate. The derivatization reaction selectively gives diastereomeric carbamates that are resolvable on an achiral non-polar GC column. The developed technique covers variously substituted THIQs, which differ significantly in volatility, steric and electronic properties. In all cases, the resolution factors (R) exceeded the value of 1.5. The method represents a robust way of analysis of mixtures of THIQs, which are often present in various matrixes such as body fluids, tissues and reaction mixtures.

A validated HPLC method for the determination of donepezil in human plasma after derivatization with 9-fluorenylmethyl chloroformate

A new HPLC method has been developed for determining donepezil in human plasma. To find the optimum conditions, a derivatization reaction was performed in different media, and the reaction product was identified by NMR and GC-MS after a semi-preparative HPLC separation. Under optimized conditions, donepezil was derivatized by 9-fluorenylmethyl chloroformate in chloroform and carbonate buffer at pH 9.5 in the presence of NaI after solid-phase extraction from a plasma sample. The reaction product was quantified on a reversed-phase TRACER EXCEL ODS-A, 5 μm column using a mixture of acetonitrile–10 mM acetate buffer(pH 6.0)–THF(60:35:5, v/v/v) as the mobile phase with fluorescence detection at 264 nm(ex) and 313 nm(em). Fluoxetine was used as the internal standard. The total run-time of the analysis was about 10 min, and a clean chromatogram was obtained. The developed method was linear over the range of 1–100 ng/mL in 500 μL of plasma samples(r2>0.998). The intra-day and inter-day precision values were in the range of 2.6%–11.6%. The limit of quantification was 1 ng/mL.

A New Initiator Cholesteryl Chloroformate for Cupper-Based Atom Transfer Radical Polymerization of Methyl Methacrylate

The polymerization of metyl methacrylate (MMA) was studied in detail by use of CuCl/L as a catalyst and cho-lesteryl chloroformate (CC) as an initiator. It was found that the atom transfer radical polymerization of MMA could proceed when L equals to a multidentate aliphatic amine ligand, N,N,N',N'',N″-penta(methyl acry-late)diethylenetriamine (MA5-DETA), and no polymerization was occurred while L=2,2'-bipyridine and 1,10- phenanthroline. The linear proportionality of the molecular weights to the conversions and straight lines observed in ln[M]0/[M] versus time plots indicated that the present polymerization system had the typical controlled polymeri-zation characteristics.

Increase in Organochlorine Contaminant Levels in Major Water Sources of the United States in Response to the Coronavirus Pandemic

Organochlorine contaminants, such as triclosan (TCS), are present in major water sources across the United States. These antimicrobial compounds are widely used as multipurpose ingredients in everyday consumer products. They can be ingested or absorbed through the skin and are found in human blood, breast milk, and urine samples. Studies have shown that the increased use of antimicrobial agents leads to their presence and persistence in the ecosystem, particularly in soil and watersheds. Many studies have highlighted emerging concerns associated with the overuse of TCS, including dermal irritations, a higher incidence of antibacterial-related allergies, microbial resistance, disruptions in the endocrine system, altered thyroid hormone activity, metabolism, and tumor metastasis and growth. Organochlorine contaminant exposures play a role in inflammatory responsiveness, and any unwarranted innate response could lead to adverse outcomes. The capacity of TCS and other organochlorine contaminants to induce inflammation, resulting in persistent and chronic inflammation, is linked to various pathologies, such as cardiovascular disease and several types of cancers. Chronic inflammation presents a severe consequence of exposure to these antimicrobial agents, as any changes could result in the loss of immune competence. Organochlorine contaminant levels were established by the United States Environmental Protection Agency (EPA) in 2019-2020 and have consistently increased in response to the novel coronavirus (nCoV) (COVID-19) pandemic. Our previous research examined the overuse of products containing triclosan (TCS), which led to an increase in total trihalomethane (TTHM) levels affecting the quality of our water supply. We also investigated the impact of the FDA ban that now requires pre-market approval. To comprehend the consequences of excessive antimicrobial use on water quality, we conducted an analysis of the levels of total trichloromethane (chloroform), a byproduct of free chlorine added to TCS, in primary water sources in metropolitan areas across the United States in 2019-2020. We repeated this analysis after the peak of the COVID-19 pandemic in 2021-2022 to examine its correlation with organochlorine exposure. Our study found that the COVID-19 pandemic, along with the increased use of antimicrobial products, has significantly raised the levels of total trihalomethanes compared to those reported in water quality reports from 2019-2020, in contrast to the reports from 2021-2022.

Genomic DNA Isolation by Phenol/Chloroform Extracting Method from Sheep Blood Clot

[ Objective] The aim was to establish the method of extracting genomic DNA from sheep blood clot on the basis of the improvement of method for extracting genomic DNA from tissues. [Method]The genomic DNA with complete primary structure and high purity was obtained from the sheep blood clot after the steps of cutting the sheep blood clot with ophthalmic scissors, cell lysis with tissue DNA extracts and digested by proteinase K, extracting with phenol/chloroform and precipitating with ethanol were performed. [ Result] The concentration of the extracted DNA was 159.90 ±0.70 ng/μl and the ratio of the A260/A280 was 1.80 ＋0.01. The sheep microsatellite locus of BM203 was amplified by using the extracted DNA from the sheep blood clot as template of PCR, and the PCR result was perfect. [Conclusion]This method is simple and feasible, the quantity and quality of the extracted DNA can satisfy the demands for the subsequent researches. It is worth to extending and using for reference.

An Application of Gas Chromatography-Mass Spectrometry (GC-MS) Fast Automated Scan/SIM Type (FASST) in Determining the Preservative Levels in Foods

The preservatives used in food products are strictly monitored and regulated. The present study aims to imply a sensitive and reliable analytical method to quantify two classes of preservatives (i.e. carboxylic acid and phenolic compounds) in food by means of gas chromatography-mass spectrometry (GC-MS), aimed at monitoring the products available within the local stores. Target analytes were derivatized via aqueous-phase isobutyl chloroformate-mediated reaction followed by dispersive liquid-liquid microextraction (DLLME) method. The quantity and quality determination of the studied samples were assured by performing FASST approach in a single run GC-MS analysis. The combination of standard addition method with sample dilution compensated the effect of sample matrix on the quantitative determination of the tested preservatives in the examined samples. The concentrations of sorbic acid (SA) were 210 μg/mL and 1000 μg/mL in soft drink and sauces samples, respectively. On the other hand, sodium benzoate (226 μg/mL) was only found in soft drink, whereas, no parabens were detected in any samples collected from the local stores.

Electron Attachment Studies for CHCl3 Using Ion Mobility Spectrometry

The dissociative electron attachment process for CHCl3 at different electric field have been studied with nitrogen as drift and carrier gas using corona discharge ionization source ion mobility spectrometry （CD-IMS）. The corresponding electron attachment rate constants varied from 1.26×10-8 cm3/（molecules s） to 8.24×10-9 cm3/（molecules s） as the electric field changed from 200 V/cm to 500 V/cm. At a fixed electric field in the drift region, the attachment rate constants are also detected at different sample concentration. The ionmolecule reaction rate constants for the further reaction between Cl^- and CHCl3 are also detected, which indicates that the technique maybe becomes a new method to research the rate constants between ions and neural molecules. And the reaction rate constants between Cl- and CHCl3 are the first time detected using CD-IMS.

Evaluation of Baishao(Radix Paeoniae Alba)and Chishao(Radix Paeoniae Rubra)from different origins based on characteristic spectra of amino acids

Objective To evaluate the difference between Baishao(Paeoniae Radix Alba,PRA)and Chishao(Paeoniae Radix Rubra,PRR)from different regions based on the characteristic spectra of amino acids(AAs).Methods Fingerprints of the 21 standard AAs were established using O-phthalaldehyde-9-fluorenylmethyl chloroformate(OPA-FMOC)pre-column derivation method.The AA components in PRA and PRR were characterized qualitatively and quantitatively,and different AAs were screened using pattern recognition technology.Results Twelve AAs were identified in both PRA and PRR.Meanwhile,aspartic acid,glutamic acid,arginine,alanine,and gamma-aminobutyric acid were screened as characteristic components,and their concentrations could effectively distinguish PRA from PRR.Conclusion The established characterization method,which is based on the characteristic spectra of AAs,is accurate,efficient,and sensitive and can effectively distinguish between PRA and PRR from different producing areas,thus providing a reference for the overall characterization and evaluation of Chinese medicinal materials.

ADSORPTION OF CHLOROFORM AND TRICHLOROETHYLENE IN WATER WITH A NEW KIND OF HYPERCROSSLINKED RESINS

In this paper two newly developed hypercrosslinked resins were used to treat micropolluted drinking water and their static and kinetic adsorption were investigated at 293 K. The results show that these two adsorbents are superior to Amberlite XAD-4 for removing chloroform and trichloroethylene in aqueous solutions. The breakthrough capacity and the total capacities from mini-column adsorption studies for chloroform and trichloroethylene on XAD-4, ZH-01 and ZH-00 are calculated respectively under experimental conditions

Chinese Medicine Formula “Shenqi San” Extract Inhibits Proliferation of Human Lung Adenocarcinoma A549 Cells via Inducing Apoptosis

The main purpose of this study was to investigate the active components of the Chinese medicine formula Shenqi San（SS） by high performance liquid chromatography with diode array detector and electrospray ionization-hybrid quadrupole time-of-flight mass spectrum（HPLC-DADESI-QTOF-MS）, and demonstrate the anticancer mechanism of SS on human lung adenocarcinoma A549 cells by evaluating the cell proliferation and apoptosis induction. The chloroform extraction of SS（CE-SS） was extracted from SS, while HPLC-DAD-ESI-QTOF-MS assay was performed to identify components of CE-SS. MTT assay was used to quantify the proliferation of A549 cells with the treatment of CE-SS. Apoptosis analysis was carried out by detecting phosphatidylserine（PS） externalization using the Annexin V-FITC Apoptosis Detection Kit and the stained cells were analyzed with a flow cytometer. DAPI staining assay was carried out to observe morphological characteristics of apoptotic cells. Western blotting was used to detect the expression of important signaling proteins including caspase-3,-8,-9, p53, Bax and Bcl-2. Eight compounds were identified through HPLC-DAD-ESI-QTOF-MS analysis and 3-pyridine carboxylic acid, barbatin C, scutebarbatine F and barbatine D might be the main compounds responsible for the antitumor effect of CE-SS. CE-SS suppressed the proliferation of lung cancer A549 cells in a time-and dose-dependent manner. By Annexin V-FITC/PI double staining, we found that treatment with CE-SS induced apoptosis in A549 cells. After 24-h exposure to CE-SS, the expression of cleaved-caspase-9, cleaved-caspase-8 and cleaved-caspase-3 protein was activated, the expression of p53 protein increased while the ratio of Bax/Bcl-2 also increased. This study identified the eight compounds of CE-SS, and demonstrated their anticancer effect on human lung adenocarcinoma A549 cells via induction of apoptosis.

Electrochemical dechlorination of chloroform in neutral aqueous solution on palladium/foam-nickel and palladium/polymeric pyrrole film/foam-nickel electrodes

Electrochemical dechlorination of chloroform in neutral aqueous solution was investigated using palladium-loaded electrodes at ambient temperature. Palladium/foam-nickel （Pd/foam-Ni） and palladium/polymeric pyrrole film/foam-nickel （Pd/PPy/foam-Ni） composite electrodes which provided catalytic surface for reductive dechlorination of chloroform in aqueous solution were prepared using an electrodepositing method. Scanning electron microscope （SEM） micrographs showed that polymeric pyrrole film modified the electrode-surface characteristics and resulted in the uniform dispersion of needle-shaped palladium particles on foam-Ni supporting electrode. The experimental results of dechlorination indicated that the removal efficiency of chloroform and current efficiency in neutral aqueous solution on Pd/PPy/foam-Ni electrode could be up to 36.8% and 33.0% at dechlorination current of 0.1 mA and dechlorination time of 180 min, which is much higher than that of Pd/foam-Ni electrode.

Prescreening teratogenic potential of chlorinated drinking water disinfection by-products by using Hydra regeneration assay

Practicability of method for the Hydra regeneration assay on the prescreening teratogenic potential of chlorinated drinking water disinfection by products was studied through both the assays of toxicity of adult Hydra (T) and inhibition of the growth of regeneration Hydra (I) by using chloroform, dichloromethane and chloroacetic acid. The results showed that T 50 / I 50 ratios of chloroform and chloroacetic acid were 2 77 and 6 16 respectively, with teratogenic potential. T 50 / I 50 ratio of dichloromethane was 1.69, with weaker teratogenic potential. These experimental results indicated preliminarily that the Hydra regeneration assay has certainly applied value as a prescreening assay for developmental toxicity.

废水中三氯乙醛分析方法研究

本文着重研究了三氯乙醛色谱分析方法,而后又与吡啶碱比色法联用,解决了汉沽工业废水中三氯乙醛和氯仿单独测定结果。此法经大量实验是可行的,摸清天津化工厂排污口三氯乙醛和氯仿总量为78.0～82.0mg/L,其中43.06～47.75mg/L为氯仿,汉沽化工厂排污口三氯乙醛和氯仿总量为5.8～6.2mg/L,其中5.56～6.00mg/L为氯仿。

Simple Modifications to Standard TRIzol®Protocol Allow High-Yield RNA Extraction from Cells on Resorbable Materials

Resorbable bioceramics are attractive for medical applications such as bone substitution. Biochemical analysis on cells cultured on these biomaterials is vital to predict the impact of the materials in vivo and RNA extraction is an essential step in gene expression study using RT-qPCR. In this study, we describe simple modifications to the TRIzol? RNA extraction protocol widely used in biology and these allow high-yield extraction of RNA from cells on resorbable calcium phosphates. Without the modifications, RNA is trapped in the co-precipitated calcium compounds, rendering TRIzol? extraction method infeasible. Among the modifications, the use of extra TRIzol? to dilute the lysate before the RNA precipitation step is critical for extraction of RNA from porous ?-tricalcium phosphate (?-TCP) discs. We also investigate the rationale behind the undesirable precipitation so as to provide clues about the modifications required for other resorbable materials with high application potential in bone tissue engineering.

Studies on the Surface Interaction and Dispersity of Silver Nanoparticles in Organic Solvents

Silver nanoparticles with different sizes have been prepared by microemulsion and have been surface-modified with C12H25SH.Electron spin resonance results indicate that there exist some kinds of surface local paramagnetic sites in capped Ag nanoparticles,which leads to the relation between electron spin resonance parameters and particle size deviating from Kawabata's description.Thereis a strong interaction between nanosilver and chloroform.The smaller the particles,the stronger the interaction.Transmission electron microscopy and ultravilolet-visible absorption spectra confirmed that Ag nanoparticles are well dispersed in chloroform,implying that a good dispersity of Ag nanoparticles in polymers could be obtained by means of solution mixing by using chloroform as the solvent.

ON THE MURPHREE EFFICIENCIES IN THE SIMULATION OF MULTICOMPONENT DISTILLATION COLUMN:THE BIZARRE BEHAVIOUR AND THE ESTIMATION METHODS

The composition profiles in an I.D.30mm Oldershaw distillation column with 6 plates at total reflux weremeasured for two ternary systems,ethanol/chloroform/n-hexane and cyclohexane/n-heptane/toluene.Somecomponent effieiencies exhibit the bizarre behaviour,exceeding the normal range(0,1),at the plates near theextreme points of the concentration profiles of the components.The possible relationship between the extremeof the profiles and the bizarre values of component efficiencies has been analysed,and the feasibility and availa-bility of some approaches for the estimation of the component efficiencies are discussed.

Chloroform Aided Extraction Spectrophotometric Determination of Rhenium Using Thiocyanate Complexing Agent

A new technique is developed for quantitative determination of rhenium in aqueous media containing molybdenum, iron and copper ions. The method seems easier and more accurate than the traditional ones. It consists of the formation of rhenium thiocyanate complex, which is extracted with chloroform at the presence of hydrochloric acid. This complex is a highly visible light absorbent that can easily be detected with the aid of a spectrophotometer. The maximum absorbance (λmax) observed for this complex was in the visible range of 430-435 nm. The experimental results showed that in a concentration range from 0.5-8 mg/L, the absorbance behavior of the rhenium thiocyanate complex is followed to the Beer-Lambert law.

Synthesis of a Novel Conjugate of Bromoarene and Polyamide Containing N-Methylimidazoles

A novel DNA cleavage conjugate of bromoarene and polyamide containing three N-methylimidazole rings was synthesized by the chloroform reaction and the DCC/HOBT coupling reaction.

An incident of chloroform poisoning on a university campus

Dear editor,University laboratory-related events include fire,explosion,chemical gas leakage,poisoning related to the loss of toxic reagents,specific pathogen infection,leakage of radioactive material,etc.[1]Chloroform is an important material used frequently in the laboratory,for organic synthesis or used as an organic glass binder and organic matter extractor.[2]As a widely used anesthetic in clinics in the 1950s and the 1960s,[3]chloroform was abandoned because of hepatorenal toxicity.We report a case of a 24-year-old suicidal female student with chloroform poisoning.

Synthesis of a Novel Conjugate of Dibenzoyldiazomethane and Polyamide Containing N-Methylimidazoles

A novel conjugate of dibenzoyldiazomethane and polyamide containing N-methylimida-zoles was synthesized by a chloroform reaction and a DCC/HOBT coupling reaction.