Polymorphism in Sulfanilamide: 14N Nuclear Quadrupole Resonance Study.

To demonstrate the selectivity of 14N nuclear quadrupole resonance (14N NQR) spectroscopy in chemistry and pharmacy, a study of sulfanilamide polymorphism was undertaken. We studied 3 known polymorphs of sulfanilamide by 14N NQR. We found at room temperature 2 sets of 3 14N NQR transition frequencies, corresponding to 2 different nitrogen sites in the crystal structure for each of 3 polymorphs. We measured the temperature dependence of all quadrupole frequencies ν+, ν-. In each set, only 1 of the 3 14N NQR frequencies is enough to characterize the polymorph. Spin-lattice relaxation time (T1) measurement is supplemental information. We also measured the transition temperature between polymorphs and estimated the ratio of polymorphs after thermal treatment of sample.

(14) N nuclear quadrupole resonance study of piroxicam: confirmation of new polymorphic form V.

A new polymorphic crystal form of piroxicam was discovered while preparing crystalline samples of piroxicam for (14) N nuclear quadrupole resonance (NQR) analysis. The new crystal form, designated as V, was prepared by evaporative recrystallization from dichloromethane. Three known polymorphic forms (I, II, and III) were also prepared. Our aim was to apply (14) N NQR to characterize the new polymorphic form of piroxicam and compare the results with those of the other known polymorphic forms. Additional analytical methods used for characterization were X-ray powder diffraction (XRPD), thermal analysis, and vibrational spectroscopy. For the first time, a complete set of nine characteristic (14) N NQR frequencies was found for each prepared polymorph of piroxicam. The consistent set of measured frequencies and calculated characteristic quadrupole parameters found for the new polymorphic form V is a convincing evidence that we are dealing with a new form. The already known piroxicam polymorphic forms were characterized similarly. The XRPD results were in accordance with the conclusions of (14) N NQR analysis. The performed study clearly demonstrates a strong potential of (14) N NQR method to be applied as a highly discriminative spectroscopic analytical tool to characterize polymorphic forms.

A miniaturized NQR spectrometer for a multi-channel NQR-based detection device.

A low frequency (0.5-5 MHz) battery operated sensitive pulsed NQR spectrometer with a transmitter power up to 5 W and a total mass of about 3 kg aimed at detecting (14)N NQR signals, predominantly of illicit materials, was designed and assembled. This spectrometer uses a standard software defined radio (SDR) platform for the data acquisition unit. Signal processing is done with the LabView Virtual instrument on a personal computer. We successfully tested the spectrometer by measuring (14)N NQR signals from aminotetrazole monohydrate (ATMH), potassium nitrate (PN), paracetamol (PCM) and trinitrotoluene (TNT). Such a spectrometer is a feasible component of a portable single or multichannel (14)N NQR based detection device.

¹4N nuclear quadrupole resonance study of polymorphism in famotidine.

(14)N nuclear quadrupole resonance (NQR) in two known polymorphs of famotidine was measured. At room temperature, seven quadrupolar sets of transition frequencies (ν(+), ν(-), and ν(0)) corresponding to seven different nitrogen sites in the crystal structure of each of the two polymorphs were found. This confirms the expected ability of NQR to distinguish polymorph B from its analog A. NQR can also measure their ratio in a solid mixture and in the final dosage form, that is, a tablet. The NQR frequencies, line shapes, and tentative assignation to all seven molecular (14)N atoms were obtained. Unravelment of these two entangled NQR spectra presents a valuable contribution to the NQR database and enables studies of some possible correlations therein. Moreover, nondestructive (14)N NQR studies of commercial famotidine tablets can reveal some details of the drug fabrication process connected with compression.

Multi-channel atomic magnetometer for magnetoencephalography: a configuration study.

Atomic magnetometers are emerging as an alternative to SQUID magnetometers for detection of biological magnetic fields. They have been used to measure both the magnetocardiography (MCG) and magnetoencephalography (MEG) signals. One of the virtues of the atomic magnetometers is their ability to operate as a multi-channel detector while using many common elements. Here we study two configurations of such a multi-channel atomic magnetometer optimized for MEG detection. We describe measurements of auditory evoked fields (AEF) from a human brain as well as localization of dipolar phantoms and auditory evoked fields. A clear N100m peak in AEF was observed with a signal-to-noise ratio of higher than 10 after averaging of 250 stimuli. Currently the intrinsic magnetic noise level is 4fTHz(-1/2) at 10Hz. We compare the performance of the two systems in regards to current source localization and discuss future development of atomic MEG systems.

Capacitor-based detection of nuclear magnetization: nuclear quadrupole resonance of surfaces.

We demonstrate excitation and detection of nuclear magnetization in a nuclear quadrupole resonance (NQR) experiment with a parallel plate capacitor, where the sample is located between the two capacitor plates and not in a coil as usually. While the sensitivity of this capacitor-based detection is found lower compared to an optimal coil-based detection of the same amount of sample, it becomes comparable in the case of very thin samples and even advantageous in the proximity of conducting bodies. This capacitor-based setup may find its application in acquisition of NQR signals from the surface layers on conducting bodies or in a portable tightly integrated nuclear magnetic resonance sensor.

Application of 14N NQR to the study of piroxicam polymorphism.

A study was conducted to test the capability of the (14)N nuclear quadrupole resonance (NQR) method to discriminate qualitatively and quantitatively among different forms of piroxicam. Samples of commercial piroxicam form I and its monohydrate were obtained on the local market. Additionally, samples of form I and II were prepared by recrystallization in 1,2-dichloroethane and ethanol, respectively. DSC and FT-IR were employed as reference methods. A (14)N NQR spectrometer was used to measure samples of different forms and mixtures of piroxicam at 2587 and 3439 kHz. DSC and FT-IR clearly confirmed differences between the different piroxicam forms. Measurements of (14)N NQR signals of different forms of piroxicam at 2587 kHz detected only spectral peaks of form I. The dependence of (14)N NQR signal intensity on the concentration of form I in mixtures with the monohydrate showed a clear linear relationship at both measured frequencies, though the scattering of data was greater at 3439 kHz due to the lower S/N ratio. The (14)N NQR method has the potential to become an additional and important spectroscopic tool in the study of solid-state forms, not only of pure active pharmaceutical ingredients or excipients, but also of their mixtures. This ability lends the method to a possible successful utilization at different levels of pharmaceutical manufacturing and product quality control.

Influence of different presentations of oscillometric data on automatic determination of systolic and diastolic pressures.

Most non-invasive blood pressure measurements are based on either the auscultatory or the oscillometric technique. In this study, we performed an extensive analysis of the signals, i.e., responses of a microphone implanted in the cuff and pressure changes in the cuff, which can be recorded during such measurements. We applied several methods to separate the cuff deflation from the arterial pressure pulses, as well as to separate the microphone data into an audible part (Korotkoff sounds) and a low frequency part. The oscillometric technique is based on some empirically derived criteria applied to the oscillometric index, which is defined as a certain characteristic physical property of pressure pulses. In addition to the pressure pulses, which are a typical physical property used for the oscillometric index, we also used in this study other properties such as a time derivative and an audible part of data measured by a microphone implanted in the cuff (Korotkoff sounds). We performed a case study of 23 healthy subjects to evaluate the influence of different presentations of the oscillometric index on known height-based and slope-based empirical algorithms for the automatic determination of the systolic and diastolic blood pressures.

Power-law correlated processes with asymmetric distributions.

Motivated by the fact that many physical systems display (i) power-law correlations together with (ii) an asymmetry in the probability distribution, we propose a stochastic process that can model both properties. The process depends on only two parameters, where one controls the scaling exponent of the power-law correlations, and the other controls the degree of asymmetry in the distributions leaving the correlations unaffected. We apply the process to air humidity data and find that the statistical properties of the process are in a good agreement with those observed in the data.