Abstract
A simple, fast, sensitive and green pretreatment method for determination of Cd, Co, Hg, Ni, Pb and V in oral and parenteral drug samples using inductively coupled plasma optical emission spectrometry (ICP OES) has been developed. According to United States Pharmacopoeia (USP), those metals must be reported in all pharmaceutical products for quality control evaluation (i.e., elemental impurities from classes 1 and 2A of USP Chapter 232). To improve the analytical capabilities of ICP OES, a dispersive liquid-liquid microextraction (DLLME) has performed using a safe, cheap and biodegradable deep eutectic solvent (DES) as extractant solvent (a mixture of 2:1 M ratio of DL-menthol and decanoic acid). Seven parameters affecting the microextraction efficiency have carefully optimized by multivariate analysis. Under optimized conditions, the DES-based DLLME-ICP OES procedure improved limit of quantitation (LOQ) values on range from 12 to 85-fold and afforded an enrichment factor on average 60-times higher than those obtained to direct ICP OES analysis. Consequently, LOQ values for Cd, Co, Hg, Ni, Pb and V have been on average 10-times lower than target limits recommended for drugs from parenteral route of administration. Trueness has evaluated by addition and recovery experiments following USP recommendations for three oral drug samples in liquid dosage form and three parenteral drugs. Recovery and RSD values have been within the range of 90–109% and 1–6%, respectively. All analytes were below the respectives LOQ values, hence, lower than the limits proposed by USP Chapter 232.
Highlights
The presence of elemental impurities as compounds in drug products can potentially have adverse health effects and must be carefully monitored
In view of the above, this study aimed to develop a simple, cheap, fast and green sample preparation procedure based on dispersive liquid-liquid microextraction (DLLME) using a synthesized deep eutectic solvent (DES) (i.e., DL-menthol and decanoic acid 2:1 M ratio) for the simultaneous extraction and preconcentration of Cd, Co, Hg, Ni, Pb, and V at trace levels from oral and parenteral drug samples for subsequent measurement by inductively coupled plasma optical emission spectrometry (ICP OES)
In the spectrum of pure decanoic acid, the COOeH and C]O vibrations were positioned at 3351 and 1727 cmÀ1, respectively. All these characteristic peaks were found in DES Fourier Transform Infrared (FT-IR) spectrum at the same position, demonstrating that the DES is comprised of DL-menthol and decanoic acid
Summary
The presence of elemental impurities as compounds in drug products can potentially have adverse health effects and must be carefully monitored. According to International Council for Harmonization of Technical Requirements for Pharmaceuticals for Human Use (ICH) [1] and USP Chapter 232 [2], permissible daily exposures (PDE) values for elemental impurities are established for pharmaceuticals from three routes of administration (i.e., oral, parenteral, and inhalational). These target elements are grouped into four main categories based on the toxicity and their likelihood of occurrence: class 1 (As, Cd, Hg, Pb), class 2A (Co, Ni, V), class 2B (Ag, Au, Ir, Os, Pd, Rh, Pt, Ru, Se, Tl), and class 3 (Ba, Cu, Cr, Li, Mo, Sb, Sn). For parenteral medications, the PDEs for the above-mentioned elements are 10-times lower and, along with elements from class 1, range from 2 to 20 mg dayÀ1 [2]
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