Quantification of coumarin in cinnamon and woodruff beverages using DIP-APCI-MS and LC-MS

The use of the direct inlet probe–atmospheric-pressure chemical ionization (DIP-APCI) ion source developed in our laboratory coupled to a high resolution Q-TOF MS for the quantitative analysis of coumarin in different cinnamon samples was demonstrated in this study. Extraction of coumarin from various cinnamon samples was followed by DIP-APCI-mass spectrometry (MS) and liquid chromatography (LC)-MS analysis. For quantification, an external calibration with and without the use of stable isotope-labeled coumarin as internal standard was compared. The results obtained by DIP-APCI-MS and LC-MS were in good agreement. Even without the use of an internal standard satisfying linearity (R ²?>?0.997), recovery (94–104 % for spiking levels between 100 and 5,000 mg/kg) and intra- and interday repeatability (2.2–13.8 %RSD) was demonstrated using DIP-APCI-MS. To reduce the number of samples requiring quantitative analysis, the possibility of semi-quantitative screening of coumarin directly from powdered cinnamon using DIP-APCI-MS was shown. The analysis of woodruff-flavored beverages and cinnamon-flavored chewing gum by DIP-APCI-MS resulted in the formation of an artifact interfering with coumarin detection. As with other ambient ionization methods, special attention has to be paid to possible spectral interferences due to isobaric substances present in the sample matrix or formed from matrix components after ionization. The temperature-programmed vaporization in DIP-APCI-MS combined with the use of stable isotope-labeled coumarin as internal standard helped in recognizing this interference.

Reactions of Podophyllotoxin with DDQ

Introduction 2, 3-Dichloro-5, 6-dicyanobenzoquinone (DDQ) can react with lignans of the mono- arylidene-butyrolactone1, aryltetralin2, dibenzylbutane3 and aryltetralin-butyrolactone4,5 series. We have studied the reactions of this reagent with podophyllotoxin 1, which is a well-known natural product on account of its long history of use in folk medicine and the biological activity of its many derivatives6. In particular, derivatives of 4-demethyl epipodophyllotoxin are used in cancer chemo…     

Light-scattering intensity fluctuations in single aerosol particles during deliquescence

We use the deliquescence of single NaCl- and NaF-particles levitated in an electrodynamic trap to study light-scattering intensity fluctuations. During deliquescence the volume of the solid crystal and the liquid around it can be measured simultaneously with the light-scattering intensity. Such an experiment allows a comparison with numerical simulations of the intensity fluctuations in microdroplets containing inclusions. We find a power-law dependence proportional to the area of the inclusion for inclusions with radii approximately less than half in size of the total radius of the droplet. For larger inclusions this changes to a power law with a proportionality to the radius of the inclusion. A change of 30% in total radius does not change the intensity fluctuations. There seems to be no distinct difference in the behaviour of NaCl and NaF particles, even though the refractive index difference between solid inclusion and liquid host is 0.165 in the former and less than 0.009 in the latter. Furthermore, the fluctuation data of the pure NaCl deliquescence is applied to the ternary NaCl–CaCl₂–H₂O system and show good agreement with thermodynamic data.     

Performance of slotted pores in particle manufacture using rotating membrane emulsification

This paper addresses the use of different slotted pores in rotating membrane emulsification technology.Pores of square and rectangular shapes were studied to understand the effect of aspect ratio (1-3.5) and their orientation on oil droplet formation.Increasing the membrane rotation speed decreased the droplet size,and the oil droplets produced were more uniform using slotted pores as compared to circular geometry.At a given rotation speed,the droplet size was mainly determined by the pore size and the fluid velocity of oil through the pore (pore fluid velocity).The ratio of droplet diameter to the equivalent diameter of the slotted pore increased with the pore fluid velocity.At a given pore fluid velocity and rotation speed,pore orientation significantly influences the droplet formation rate: horizontally disposed pores (with their longer side perpendicular to the membrane axis) generate droplets at double the rate of vertically disposed pores.This work indicates practical benefits in the use of slotted membranes over conventional methods.     

Monolithic circuits with epitaxial graphene/silicon carbide transistors

A concept is presented that uses epitaxial graphene on silicon carbide (SiC) for digital circuits. It uses graphene as a metal and the underlying substrate SiC as semiconductor. On the base of transistors with excellent switching behavior, Inverter and NAND operation is demonstrated.

     

Light- and Manganese-Initiated Borylation of Aryl Diazonium Salts: Mechanistic Insight on the Ultrafast Time-Scale Revealed by Time-Resolved Spectroscopic Analysis

Manganese-mediated borylation of aryl/heteroaryl diazonium salts emerges as a general and versatile synthetic methodology for the synthesis of the corresponding boronate esters. The reaction proved an ideal testing ground for delineating the Mn species responsible for the photochemical reaction processes, that is, involving either Mn radical or Mn cationic species, which is dependent on the presence of a suitably strong oxidant. Our findings are important for a plethora of processes employing Mn-containing carbonyl species as initiators and/or catalysts, which have considerable potential in synthetic applications.     

What is the recall rate of breast MRI when used for screening asymptomatic women at high risk?

Breast screening acceptability is dependent on sensitivity and recall rate. We aimed to establish the recall rate for MRI and mammography, separately and together, when screening a cohort of women at high genetic risk. Women aged 35-49 years in the MARIBS study form the cohort. We analysed the recall rate, the number of extra tests and their effectiveness. Wilcoxon Rank test was used to estimate the effect of age and logistic regression with robust variance the effect of mammographic density on recall rates. The first 726 screening studies took place in 415 women. Following 86 of these recall occurred, comprising 140 additional investigations. 28 of the cases were resolved without further MRI, and 18 women had more than 2 additional tests. Neither age nor mammographic density was associated with recall. MRI had a recall of rate of 10.19%, and mammography 4.00%. The two techniques largely recalled different cases and 10 cases only (11.62% of those recalled) were abnormal by both tests. The two together had a recall rate of 11.85%. Recall rates varied widely between centres of the study. Breast MRI in asymptomatic high-risk women age 35-49 years largely recalls different women from mammography. The combined figure of approximately 12% may be acceptable for screening and will be useful for planning similar studies.     

A HYPERBOLIC SYSTEM OF CONSERVATION LAWS FOR FLUID FLOWS THROUGH COMPLIANT AXISYMMETRIC VESSELS

We are concerned with the derivation and analysis of one-dimensional hyperbolic systems of conservation laws modelling fluid flows such as the blood flow through compliant axisymmetric vessels.Early models derived are nonconservative and/or nonhomogeneous with measure source terms,which are endowed with infinitely many Riemann solutions for some Riemann data.In this paper,we derive a one-dimensional hyperbolic system that is conservative and homogeneous.Moreover,there exists a unique global Riemann solution for the Riemann problem for two vessels with arbitrarily large Riemann data,under a natural stability entropy criterion.The Riemann solutions may consist of four waves for some cases.The system can also be written as a 3×3 system for which strict hyperbolicity fails and the standing waves can be regarded as the contact discontinuities corresponding to the second family with zero eigenvalue.