HPLC-MS/MS method validation for the detection of carbadox and olaquindox in poultry and swine feedingstuffs

Abstract

Carbadox (CBX) and olaquindox (OLA) were used in poultry and swine feed for growth promotion, to improve feed efficiency and increase the rate of weight gain. However, the use of these agents in feedingstuffs was prohibited because of concerns about their toxicity. Regulatory laboratories are required to have suitably validated analytical methods to ensure compliance with the ban. A quantitative and confirmatory method for determining the presence of CBX and OLA in poultry and swine feed by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was developed, optimized, and validated. The analytes extraction was performed with a mixture of water and acetonitrile (1:1v/v) and cleanup with hexane and C18 (dispersive phase). The method was evaluated by the following parameters: specificity, linearity, matrix effect, decision limits (CCα), detection capability (CCβ), accuracy, precision, limits of detection (LoD), limits of quantification (LoQ) and measurement uncertainty. The validated method presented a broad linear study range and no significant matrix effect. The limit of detection (LoD) was defined at 9 μg kg(-1) for CBX and 80 μg kg(-1) for OLA, and the limit of quantification (LoQ) was defined at 12 μg kg(-1) and 110 μg kg(-1) for CBX and OLA, respectively. The accuracy of the method was adequate for CBX and OLA. The recovery values found in the repeatability conditions were 99.41% for CBX and 104.62% for OLA. Under intralaboratory reproducibility conditions, the values were 98.63% for CBX and 95.07% for OLA. It was concluded that the performance parameters demonstrated total method adequacy for the detection and quantification of CBX and OLA in poultry and swine feedingstuffs.

Tracking toxic hypoglycin A over two maturity stages of different positions in four Chinese litchi cultivars by UPLC-MS/MS

“…Sensitivity was estimated by LOD and LOQ, the amount of LOD was three times as much as the peak height of baseline background, while for LOQ, it was ten times. LOD and LOQ can also be calculated through the slope of linear equation and the standard deviation of noise of the baseline background, the equation as follow [29].…”

Hydrophilic‐interaction‐based magnetically assisted matrix solid‐phase dispersion extraction of carbadox and olaquindox in feeds

“…As a solid sample, feed is often subjected to liquid–liquid extraction (LLE), solid‐phase extraction (SPE)/molecularly imprinted SPE, and high‐performance liquid chromatography (HPLC) coupled with an ultraviolet (UV) detection or tandem mass spectrometry (MS/MS) for the extraction, purification, and determination of carbadox and olaquindox 4‐8 . For example, carbadox and olaquindox could be extracted by methanol–acetonitrile (ACN)–water with ultrasonic assistance, then dried and redissolved in monopotassium phosphate solution, purified by Oasis® HLB‐based SPE, and finally dried again and redissolved in the initial mobile phase 4 .…”

Novel Electrochemical Sensor Fabricated for Individual and Simultaneous Ultrasensitive Determination of Olaquindox and Carbadox Based on MWCNT-OH/CMK-8 Hybrid Nanocomposite Film

“…Many methods, such as high-performance liquid chromatography (HPLC) [14,15,16], HPLC with mass spectrometry [17,18,19,20], gas chromatography mass spectrometry [12], and immunosorbent assay, have been developed to detect quinoxalines and their metabolites [9,21,22]. However, these methods require expensive equipment, complicated and time-consuming sample preparation processes, and highly skilled personnel and technicians, and thus are limitedly applied.…”