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.

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.

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.

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.

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.

A NEW ROUTE FROM HETEROAROMATIC BORON COMPOUNDS TO CORRESPONDING KETONES VIA DICHLOROCARBENE INSERTION UNDER PHASE TRANSFER CONDITIONS

The reactions of tri-2-benzofuranylborane or aminoethyl di-2-thienylborinate and 2-thienylphenylborinate with dichlorocarbene generated in situ from chloroform under phase transfer conditions were explored as a new route for the preparation of heteroaromatic ketones. It was found that a good yield of the ketones can be obtained by solid-liquid system.

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.

PREPARATION AND PERVAPORATION PROPERTIES OF PROPENE/1-DECENE COPOLYMER MEMBRANES

Propene/1-decene copolymers （P-co-D） were synthesized by means of slurry polymerization process under atmospheric pressure using Ziegler-Natta catalyst （MgCl2/TiCl4/AlEt3）. The random P-co-Ds were elastic, low-crystalline, thermally stable and therefore suitable to be used as membrane materials in organophilic pervaporation with chloroform/water mixture. Its mechanical strength is better than polydimethylsiloxane （PDMS）. The correlation between structural parameters （glass transition temperature and crystallinity） and properties of organophilic pervaporation were investigated.

Studies on the Analgesic Activity and Acute Toxicities of Bidens alba(L.) DC

[Objectives]This study was conducted to investigate the analgesic effects and acute toxicities of Bidens alba (L.) DC.[Methods]The alcohol extract of B.alba (L.) DC was extracted and separated with petroleum ether and chloroform successively.The acute toxicities of the two extracts on mice were measured,and then the analgesic effects were measured with writhing pain model induced by acetic acid.[Results]No mice died when the crude dosages of B.alba (L.) DC from petroleum ether extract and chloroform extract were 5 016 and 5 100 mg/kg,respectively.When the petroleum ether extract was 60.0 mg/kg,the percentage of twisted mice induced by acetic acid was 40%,the analgesic rate was 77.5%,and the time of the first writhing was (294.0±165.8) s;when the chloroform extract was 20.0 mg/kg,the percentage of twisted animals was 55.6%,the analgesic rate was 51.5%,and the time of the first writhing was (273.8 ±153.4) s;and when the chloroform extract was 4.0 mg/kg,the percentage of twisted animals was 40%,and the analgesic rate was 62.1%,and the time of the first writhing was (370.6±231.3) s.[Conclusions]The petroleum ether extracts and chloroform extracts of B.alba (L.) DC have good analgesic effects and no acute toxicities.