Nuclear Quadrupole Resonance: A Technique to Control Hydration Processes in the Pharmaceutical Industry

Limandri, Silvina P.; Visñovezky, Claudia; Pérez, S.C.; Schürrer, Clemar; Wolfenson, A. E.; Ferro, Maribel; Cuffini, Silvia Lucía; Souza, J. C.; Aguiar, Fernando Nalesso; Gaitani, Cristiane Masetto de

doi:10.1021/ac103106y

Cited by 15 publications

(12 citation statements)

References 15 publications

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“…A similar investigation for the antidiabetic drug diabinese can be found in References [11]. In Reference [12] the authors show the clear distinguishability of differently hydrated species of diclofenac preparations and confirm the usefulness of NQRS for hydration monitoring of drug compounds containing quadrupolar nuclei. An application with high potential impact is the detection of explosives, as important compounds like Trinitrotoluene (TNT) and Cyclotrimethylenetrinitramine, commonly labelled as RDX, have very characteristic NQR fingerprints, see, for example, References [13,14].…”

Section: Introductionsupporting

confidence: 57%

Tris(2-Methoxyphenyl)Bismuthine Polymorphism Characterized by Nuclear Quadrupole Resonance Spectroscopy

et al. 2019

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Based on the previous identification of metastable polymorphs in crystalline triphenylbismuth by nuclear quadrupole resonance spectroscopy (NQRS), the potential formation of similar phases was studied in Tris(2-Methoxyphenyl)Bismuthine. To this end, commercial samples with known NQRS properties were molten and re-crystallized at different speeds (shock freezing in different coolants versus slow cooling inside of a heater). In all recrystallization products we have identified a new crystal phase which has not been observed after synthesis from a solution. The new crystallographic structure has been confirmed by X-ray diffraction (XRD). The newly isolated polymorph crystallizes in the monoclinic space group P2(1)/c with only one molecule in the asymmetric unit and consequently only one 5/2-7/2 transition is observed at 88.75 MHz at 310 K. In contrast, the two transitions at 89.38 and 89.29 MHz for the well-known trigonal polymorph originate from two crystallographically distinct molecules of Tris(2-methoxy-Phenyl)Bismuthine in the asymmetric unit. Additional relaxometric NQRS shows distinctly different T2 relaxation times for the new polymorph when compared to the original samples. Additional phase transitions could not be observed during temperature sweeps between 153K and 323K.

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Section: Introductionsupporting

confidence: 57%

Tris(2-Methoxyphenyl)Bismuthine Polymorphism Characterized by Nuclear Quadrupole Resonance Spectroscopy

et al. 2019

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“…In a recent publication, Limandri et al demonstrated that nuclear quadrupole resonance (NQR) spectroscopy is also a useful tool to identify hydrates and also monitor hydration dynamics. NQR is otherwise known to be able to identify and quantify different polymorphs in pharmaceutical agents. − The NQR spectrum is typically simple, i.e.…”

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confidence: 99%

Quantitative Analysis of Hydration Using Nitrogen-14 Nuclear Quadrupole Resonance

Gregorovič

2015

Anal. Chem.

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Hydration is a quite common process in pharmaceutical solids. Sometimes it is desirable, as it stabilizes the crystal structure; in other cases it is unwanted, as it changes the physical and chemical properties of drugs. We here use (14)N NQR spectroscopy to quantitatively analyze hydration of a model compound, 5-aminotetrazole. (14)N NQR has some great advantages compared to other routinely used techniques to study hydration, like a very simple spectrum, single point calibration, and no need for special sample preparation, but the method's great disadvantage is a rather small sensitivity. Nevertheless, here we demonstrate that (14)N NQR, although being significantly less sensitive than XRD, NIR, and also (35)Cl NQR, is still capable of providing excellent quantitative accuracies. We can achieve errors <1% of the total amount, provided good temperature stabilization is implemented, which then allows long experimental times. We also present results obtained with a SLSE pulse sequence, which is a less robust approach but allows the use of much shorter measuring times (∼200×) and could be used for quantitative real time monitoring of hydration or dehydration.

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“…surroundings for the α-and β-polymorphs via the spin-lattice relaxation time, , measurements is additional information. It is a valuable supplement to the 13 C and 15 N NMR magic angle spinning data (chemical shifts) as well as the corresponding data for all three polymorphs [40]. Article [25] concludes with " 14 N NQR studies demonstrate that we were dealing with the room temperature stable forms of all three polymorphs.…”

Section: N Nqr In Sulfanilamidementioning

confidence: 99%

“…The view into the lattice dynamics of the N(1) and N(2) nitrogen atoms and their surroundings for the αand β-polymorphs via the spin-lattice relaxation time, T 1 , measurements is additional information. It is a valuable supplement to the 13 C and 15 N NMR magic angle spinning data (chemical shifts) as well as the corresponding T 1 data for all three polymorphs [40].…”

Section: N Nqr In Sulfanilamidementioning

confidence: 99%

“…Like NMR, NQR is a quantitative method, meaning that the given signal intensity is proportional to the number of nuclei with the corresponding resonance frequency. Since, for example, the hydration of a substance significantly shifts the resonance, it is possible to monitor the hydration process, as recently demonstrated both by 35 Cl NQR [13] and 14 N NQR [14].…”

Section: Introductionmentioning

confidence: 99%

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Nuclear Quadrupole Resonance (NQR)—A Useful Spectroscopic Tool in Pharmacy for the Study of Polymorphism

et al. 2020

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Nuclear Quadrupole Resonance (NQR) spectroscopy has been known for 70 years. It is suitable for the study of measured (poly)crystalline chemical compounds containing quadrupole nuclei (nuclei with spin I ≥ 1) where the characteristic NQR frequencies represent the fingerprints of these compounds. In several cases, 14N NQR can distinguish between the polymorphic crystalline phases of active pharmaceutical ingredients (APIs). In order to further stimulate 14N NQR studies, we review here several results of API polymorphism studies obtained in Ljubljana laboratories: (a) In sulfanilamide, a clear distinction between three known polymorphs (α, β, γ) was demonstrated. (b) In famotidine, the full spectra of all seven different nitrogen positions were measured; two polymorphs were distinguished. (c) In piroxicam, the 14N NQR data helped in confirming the new polymorphic form V. (d) The compaction pressure in the tablet production of paracetamol, which is connected with linewidth change, can be used to distinguish between producers of paracetamol. We established that paracetamol in the tablets of six different manufacturers can be identified by 14N NQR linewidth. (e) Finally, in order to get an extremely sensitive 14N NQR spectrometer, the optical detection of the 14N NQR signal is mentioned.

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Nuclear Quadrupole Resonance: A Technique to Control Hydration Processes in the Pharmaceutical Industry

Cited by 15 publications

References 15 publications

Tris(2-Methoxyphenyl)Bismuthine Polymorphism Characterized by Nuclear Quadrupole Resonance Spectroscopy

Tris(2-Methoxyphenyl)Bismuthine Polymorphism Characterized by Nuclear Quadrupole Resonance Spectroscopy

Quantitative Analysis of Hydration Using Nitrogen-14 Nuclear Quadrupole Resonance

Nuclear Quadrupole Resonance (NQR)—A Useful Spectroscopic Tool in Pharmacy for the Study of Polymorphism

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