Development and Validation of an HPLC Method for the Analysis of Chlorpropham and 3-Chloroaniline in Potato Extracts

Abstract

Chlorpropham (CIPC) is the main sprout inhibitor used by potato industry. There is concern about the residues of CIPC and its degradation product 3-chloroaniline, 3-CA; hence, analytical methods are required to analyse their residues in potato samples. An HPLC-UV method was developed and validated for the separation and quantification of these compounds using propham (IPC) as an internal standard. The chromatographic conditions required to achieve good separation were 60% mobile phase of methanol, 15-minute run time at a flow rate of 1.5 mL/min, and a detection wavelength of 210 nm using Phenomenex (ODS-2 250 mm×4.60 mm 5 µm Sphereclone) column at an ambient temperature. The method was validated for precision, linearity, the limit of detection (LOD) and the limit of quantification (LOQ), producing high precision through RSD ≤ 0.03%, and acceptable criteria of the coefficient of determination (R2) of the calibration curves (0.990). LOD values of CIPC and 3-CA were approximately 0.01 µg/mL whereas the LOQ values were approximately 0.04 µg/mL using repeated injection approach. The proposed HPLC method was compared with the standard GC method of the CIPC residues extracted showing good agreementR2=0.99. Despite using the same extract, the recovery results for the proposed HPLC method were 13% higher than GC analysis.

Determination of chlorpropham (CIPC) residues, in the concrete flooring of potato stores, using quantitative (HPLC UV/VIS) and qualitative (GCMS) methods

“…Extracted industrial concrete samples were diluted to fit this concentration range prior to analysis (Figure 2). Sensitivity was evaluated by estimating the limit of quantification (LOQ) and limit of detection (LOD) using a repeat injection method (n=10) (Mohammed et al, 2014). The LOD and LOQ values, with respect to the instrument response to CIPC, were evaluated using 0.01 µg mL -1 CIPC solutions.…”

“…Boyd and Duncan (1986b) reported on the accumulation of CIPC residues in the concrete structures of a potato store and demonstrated concentrations in the concrete walls and flooring in the range of 130-290 mg kg -1 and 2050-9470 mg kg -1 , respectively. However, this method involved time-consuming Soxhlet extraction followed by a flame ionisation detection (GC-FID) method which is less sensitive for CIPC compared to other methods such as HPLC UV/VIS (Mohammed, 2014). Therefore, alternative, higher sensitivity analytical methods are required to detect CIPC in building materials, to allow informed recommendations to be made to farmers about the re-use of stores for other crop commodities.…”

Sprout suppression on potato: need to look beyond CIPC for more effective and safer alternatives

“…One of such breakdown product of CIPC is 3-chloroaniline (3-CA) and being aniline based derivative this is considered more polluting and highly toxic than the parent compound itself (Park 2004;Orejuela and Silva 2005;Balaji et al 2006;Sihtmaee et al 2010;Smith and Bucher 2012). As per Mohammed et al (2014Mohammed et al ( , 2015, 3-CA is aromatic amine and dangerous to human and environment. The potential/possible danger with respect to 3-CA can be realized from the fact that other 2 derivatives of aniline i.e., 2-chloroaniline and 4-chloroaniline are already classified as hazardous substances which are possibly carcinogenic to humans (Sihtmaee et al 2010;Smith and Bucher 2012).…”

Fate of Chlorpropham during High-Temperature Processing of Potatoes

“…However, as the results of standard hydrolysis experiments (OECD 507) indicated the formation of 3-chloroaniline, the consideration of processed food could potentially increase the exposure to 3-chloroaniline and the exceedance of ARfD and ADI values . While its toxicological potential has been extensively discussed in the past, ,− EFSA assumed 3-chloroaniline unlikely to be genotoxic in 2017 . The current EU residue definition for risk assessment of chlorpropham in plant commodities includes the active substance itself, 4′-hydroxychlorpropham (free and conjugated) and 3-chloroaniline (free and conjugated).…”