Syringe‐to‐syringe dispersive liquid‐phase microextraction solidified floating organic drop combined with high‐performance liquid chromatography for the separation and quantification of ochratoxin A in food samples
Abstract:A new, simple, and rapid syringe-to-syringe dispersive liquid-phase microextraction with solidified floating organic drop was used for the separation and preconcentration of ochratoxin A from grain and juice samples before its quantification using high-performance liquid chromatography and fluorescence detection. Factors influencing the microextraction efficiency of ochratoxin A, such as sample solution pH, type and volume of organic extractant, salt concentration, number of injections, and volume of the sampl… Show more
“…Salt addition might pose double effects on the LPME extraction efficiency of target analytes, such as decreasing the solubility of analytes and acceptor phase by salting‐out effect, reducing the diffusion coefficients of analytes . A mass of optimization experiments have showed that NaCl addition does not have an important effect on the LPME efficiencies of analytes such as ochratoxin , albendazole and triclabendazole , or even a considerable negative effect on the extraction efficiency of some pesticide residues in fruit and vegetable samples . Although the addition of salt such as saturated Na 2 SO 4 did increase the extraction efficiency of SAs , there was no further optimization of salt effect in the present study.…”
Section: Resultsmentioning
confidence: 99%
“…The adjusted filtrate was spiked with a concentration of 0.1 or 5 μg/L of each SA for recovery testing and simultaneously spiked with SNA at 0.5 μg/L as external standard . The enrichment factor (EF) and extraction recovery (%) of the method were calculated by the following equations: where C a and C w are, respectively, the level of SAs in the organic extractant after extraction by the developed method and the level of SAs in the aqueous sample without extraction, V organic and V aqueous are the volume of the organic extractant and the volume of the aqueous sample, respectively . The precision of this method was expressed as the RSD of triplicate measurements.…”
Section: Methodsmentioning
confidence: 99%
“…where C a and C w are, respectively, the level of SAs in the organic extractant after extraction by the developed method and the level of SAs in the aqueous sample without extraction, V organic and V aqueous are the volume of the organic extractant and the volume of the aqueous sample, respectively [49]. The precision of this method was expressed as the RSD of triplicate measurements.…”
A sensitive method for determining sulfonamides in water was developed and validated through in situ derivatization and hollow-fiber liquid-phase microextraction with ultra-high performance liquid chromatography and fluorescence detection. The target sulfonamides were sulfadiazine, sulfacetamide, sulfamerazine, sulfamethazine, sulfamethoxypyridazine, sulfachloropyridazine, sulfamethoxazole, and sulfisoxazole. Following in situ derivatization with fluorescamine, three-phase hollow-fiber liquid-phase microextraction with an S 6/2 polypropylene hollow-fiber membrane was applied automatically using a multipurpose autosampler. Experimental parameters including derivatization time, choice of organic phase, pH of donor and acceptor phase, stirring rate, extraction temperature and time were optimized. Under optimized conditions, the target sulfonamides achieved excellent linearity with correlation coefficients of 0.9924-0.9994 within the concentration range of 0.05-5 μg/L. The limits of detection of the eight sulfonamides were 3.1-11.2 ng/L, and the limits of quantification were 10.3-37.3 ng/L. Enrichment factors of 0.1 and 5 μg/L sulfonamides spiked in lake water were 14-60, and recoveries were 56-113% with relative standard derivations of 3-19%. Applied with the developed method, sulfamerazine and sulfamethoxazole were measurable in both influent and effluent water of the three sewage treatment plants in Guangzhou, China. The developed method was sensitive and provided an alternative method for simultaneously enriching and quantifying multiple sulfonamides in environmental water.
“…Salt addition might pose double effects on the LPME extraction efficiency of target analytes, such as decreasing the solubility of analytes and acceptor phase by salting‐out effect, reducing the diffusion coefficients of analytes . A mass of optimization experiments have showed that NaCl addition does not have an important effect on the LPME efficiencies of analytes such as ochratoxin , albendazole and triclabendazole , or even a considerable negative effect on the extraction efficiency of some pesticide residues in fruit and vegetable samples . Although the addition of salt such as saturated Na 2 SO 4 did increase the extraction efficiency of SAs , there was no further optimization of salt effect in the present study.…”
Section: Resultsmentioning
confidence: 99%
“…The adjusted filtrate was spiked with a concentration of 0.1 or 5 μg/L of each SA for recovery testing and simultaneously spiked with SNA at 0.5 μg/L as external standard . The enrichment factor (EF) and extraction recovery (%) of the method were calculated by the following equations: where C a and C w are, respectively, the level of SAs in the organic extractant after extraction by the developed method and the level of SAs in the aqueous sample without extraction, V organic and V aqueous are the volume of the organic extractant and the volume of the aqueous sample, respectively . The precision of this method was expressed as the RSD of triplicate measurements.…”
Section: Methodsmentioning
confidence: 99%
“…where C a and C w are, respectively, the level of SAs in the organic extractant after extraction by the developed method and the level of SAs in the aqueous sample without extraction, V organic and V aqueous are the volume of the organic extractant and the volume of the aqueous sample, respectively [49]. The precision of this method was expressed as the RSD of triplicate measurements.…”
A sensitive method for determining sulfonamides in water was developed and validated through in situ derivatization and hollow-fiber liquid-phase microextraction with ultra-high performance liquid chromatography and fluorescence detection. The target sulfonamides were sulfadiazine, sulfacetamide, sulfamerazine, sulfamethazine, sulfamethoxypyridazine, sulfachloropyridazine, sulfamethoxazole, and sulfisoxazole. Following in situ derivatization with fluorescamine, three-phase hollow-fiber liquid-phase microextraction with an S 6/2 polypropylene hollow-fiber membrane was applied automatically using a multipurpose autosampler. Experimental parameters including derivatization time, choice of organic phase, pH of donor and acceptor phase, stirring rate, extraction temperature and time were optimized. Under optimized conditions, the target sulfonamides achieved excellent linearity with correlation coefficients of 0.9924-0.9994 within the concentration range of 0.05-5 μg/L. The limits of detection of the eight sulfonamides were 3.1-11.2 ng/L, and the limits of quantification were 10.3-37.3 ng/L. Enrichment factors of 0.1 and 5 μg/L sulfonamides spiked in lake water were 14-60, and recoveries were 56-113% with relative standard derivations of 3-19%. Applied with the developed method, sulfamerazine and sulfamethoxazole were measurable in both influent and effluent water of the three sewage treatment plants in Guangzhou, China. The developed method was sensitive and provided an alternative method for simultaneously enriching and quantifying multiple sulfonamides in environmental water.
“…Recently, SFODME has been helpful for the identification of phenytoin and phenobarbital in plasma and urine samples [ 79 ]. Currently, an easy and fast syringe-to-syringe dispersive liquid-phase microextraction method with SFO drops has been developed and is useful for the analysis of ochratoxin-A [ 80 ], mercury in fish samples [ 81 ], and naproxen in plasma [ 82 ]. Fig.…”
Section: Sample Preparation Techniques In Bioanalyticsmentioning
“…Thus, LPME as a miniaturized form of LLE is introduced to eliminate these limitations. LPME is carried out in various shapes including single drop microextraction [12], dispersive liquid-liquid microextraction (DLLME) [13,14], and hollow fiber LPME [15,16]. Among them, DLLME is widely used for the separation of various analytes from different samples because it has several good advantages such as having a simple and rapid procedure, and high enhancement factor [13,17].…”
A simple and rapid in‐syringe vortex‐assisted emulsification microextraction with solidified floating organic drop was developed for the extraction of aflatoxins (B1 and B2) from feed before their determined by high‐performance liquid chromatography. Several experimental factors affect the microextraction efficiency such as sample pH, vortex time, type of extraction solvent, and sample volume that have been evaluated and optimized. The calibration curves were linear in the range of 50.0–500.0 and 40.0–400.0 ng kg−1 for aflatoxin B1 and aflatoxin B2, respectively. The limits of detection were found to be 16.0 and 12.0 ng kg−1 for aflatoxin B1 and aflatoxin B2, respectively. The inter‐day and intra‐day precisions of the developed method were in the range of 5.3–9.3%. Finally, the developed microextraction method was successfully used in the extraction and quantification of aflatoxins in several feed samples.
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