title: An optimized and validated (1)H NMR method for the quantification of α-pinene in essentials oils.
abstract: The authenticity and composition of commercial essential oils requires strict quality control. Due to the importance of α-pinene containing essential oils, a rapid and efficient method for quantification of this terpene in oils of eucalyptus, pink pepper and turpentine using (1)H NMR was developed and validated. All evaluated parameters (selectivity, linearity, accuracy/precision, repeatability, robustness, stability of analyte and internal standard in solutions) showed satisfactory results. The limit of detection (LOD) and limit of quantification (LOQ) were 0.1 and 2.5mg respectively. These values indicated that α-pinene was detected in 35 mg samples containing at least 0.3% of this compound. In addition, a minimum of 8% of α-pinene in the sample was required for quantification. Furthermore, the standard deviations found in the (1)H NMR methodology were less than 1% and were lower than those obtained by gas chromatographic analysis. Statistical tests have shown that the results obtained by (1)H NMR methodology are similar to those obtained by GC-FID technique using external and internal standardization and normalization within 95% confidence. R&R values lower than 10% have shown that all the methods are appropriate and the (1)H NMR method is suitable for quantification of α-pinene in samples of essential oils since this method possessed the smallest R&R (1.81) value.
authors.affiliation: Departamento de Química, Universidade Federal de Viçosa, Av. Peter Henry Holfs, S/N, Viçosa, MG 36570-900, Brazil.
authors.forename: Cristiane I
authors.initials: CI
authors.lastname: Cerceau
authors.affiliation: Departamento de Química, Universidade Federal de Viçosa, Av. Peter Henry Holfs, S/N, Viçosa, MG 36570-900, Brazil; Departamento de Química, Instituto de Ciências Exatas, Universidade Federal de Minas Gerais, Av. Pres. Antônio Carlos, 6627, Campus Pampulha, Belo Horizonte, MG 31270-901, Brazil. Electronic address: lcab@ufmg.br.
authors.forename: Luiz C A
authors.initials: LC
authors.lastname: Barbosa
authors.affiliation: Departamento de Química, Universidade Federal de Viçosa, Av. Peter Henry Holfs, S/N, Viçosa, MG 36570-900, Brazil.
authors.forename: Claudinei A
authors.initials: CA
authors.lastname: Filomeno
authors.affiliation: Departamento de Química, Universidade Federal de Viçosa, Av. Peter Henry Holfs, S/N, Viçosa, MG 36570-900, Brazil.
authors.forename: Elson S
authors.initials: ES
authors.lastname: Alvarenga
authors.affiliation: Departamento de Química, Universidade Federal de Viçosa, Av. Peter Henry Holfs, S/N, Viçosa, MG 36570-900, Brazil.
authors.forename: Antônio J
authors.initials: AJ
authors.lastname: Demuner
authors.affiliation: Departamento de Química, Universidade Federal do Jequitinhonha e Mucuri, Campus JK, 39100-000 Diamantina, MG, Brazil.
authors.forename: Paulo H
authors.initials: PH
authors.lastname: Fidencio
mesh_terms: D000081008:Bicyclic Monoterpenes; D008401:Gas Chromatography-Mass Spectrometry; D057230:Limit of Detection; D016014:Linear Models; D009682:Magnetic Resonance Spectroscopy / Q000379:methods*; D039821:Monoterpenes / Q000032:analysis* / Q000737:chemistry; D009822:Oils, Volatile / Q000737:chemistry*; D011786:Quality Control; D013997:Time Factors
chemical_list: D000081008:Bicyclic Monoterpenes; D039821:Monoterpenes; D009822:Oils, Volatile; C005451:alpha-pinene
keywords: Essential oils; Gas chromatography; Quantitative nuclear magnetic resonance; α-Pinene.