Rapid detection of black pepper adulteration withendogenous and exogenous materials : assessment of benchtop and handheld infrared spectrometers

Abstract

Black pepper is the most widely used spice crop globally and has significant economic value, making it a target for economically motivated adulteration. A wide range of organic and inorganic bulking materials has been used as adulterants in black pepper. Development of rapid non-targeted screening methods for use at different stages of the black pepper supply chain is extremely important for the identification and prevention of evolving fraudulent practices. This study has assessed the potential of benchtop Fourier Transform infrared with attenuated total reflectance (FTIR-ATR), benchtop Fourier Transform near-infrared (FT-NIR), and two handheld NIR spectrometers, coupled with chemometrics, for the discrimination of black pepper (Piper nigrum), pepper from other species and genera (non- Piper nigrum) and a broad range (n = 27) of endogenous and exogenous adulterants. Spiked samples were prepared to imitate pepper adulteration with seven different adulterants at five levels of adulteration (5%, 25%, 50%, 75%, 95% w/w). Orthogonal partial least squares discriminant analysis (OPLS-DA) achieved 100% total prediction accuracy for both FTIRATR and FT-NIR in differentiating authentic Piper nigrum and adulterant samples. The handheld microNIR 1700ES resulted in a 91.30% correct classification rate, while the SCiO model achieved 86.96% prediction accuracy. Detection of black pepper adulteration with multiple adulterants was performed using data-driven soft independent modelling of class analogy (DD-SIMCA). The highest performance of the DD-SIMCA model was achieved by FTIR-ATR (100% sensitivity and 100% specificity) followed by FT-NIR (98% sensitivity and 99% specificity). The handheld microNIR 1700ES resulted in 95% sensitivity and 90% specificity. This study demonstrated that FTIR-ATR and FT-NIR, coupled with DD-SIMCA, can effectively detect black pepper adulteration with multiple endogenous and exogenous adulterants. The handheld NIR (microNIR1700ES) clearly demonstrated the potential for rapid and effective verification of Piper nigrum authenticity outside the laboratory.