Mao J.,Laboratory of Quality and Safety Risk Assessment for Agro Products Chengdu |
Lei S.,Laboratory of Quality and Safety Risk Assessment for Agro Products Chengdu |
Xiao D.,University of Sichuan |
Fu C.,Laboratory of Quality and Safety Risk Assessment for Agro Products Chengdu |
And 2 more authors.
Food Control | Year: 2014
The immunoaffinity column cleanup method coupled with HPLC separation and fluorescence detection is still one of the most frequently used quantitative methods for routine analyses of AFM1. In this study, aflatoxin M1 (AFM1) was quantified with a chromatography column packed with 2.6μm core-shell particles on a conventional HPLC. A large volume of solvent (100μL) was injected into the highly efficient column without any noticeable reduction in separation performance with the help of stepwise gradient elution. The instrumental conditions were optimized by response surface analysis methodology (RSM) with a three-level three-factor Box-Behnken design. The use of core-shell columns on conventional HPLC for AFM1 analysis under the optimized instrumental conditions leads to increased analytical performance compared with traditional totally porous columns without the heavy costs associated ultra-high-pressure instruments. Moreover, the improved instrumental sensitivity enables simplified sample preparation by avoiding any solvent replacement. The method could be easily applied to enhance the sensitivity of HPLC-FLD for AFM1 analysis that is based on isocratic elution and is more widely used. The method was successfully applied to 40 raw milk samples collected in summer from 20 cattle ranches located in two different provinces in southwestern China. © 2014 Elsevier Ltd.
Mao J.,Academy of Agricultural Science |
Mao J.,Laboratory of Quality and Safety Risk Assessment for Agro products Chengdu |
Mao J.,University of Sichuan |
Lei S.,Academy of Agricultural Science |
And 4 more authors.
Food Control | Year: 2013
Ochratoxin A (OTA) is a mycotoxin commonly present in red wine and other foodstuffs. It is widely studied due to its nephrotoxic, immunotoxic, teratogenic and carcinogenic effects. Nowadays, liquid chromatography is the main method for OTA analysis. With the recent development on the column technology, core-shell columns were commercialized in recent years. It is with high performance while maintain low back pressure thus could be used on conventional HPLC instrument. However, as current conventional benchmark high-performance liquid chromatographs were not initially designed for the recently developed high-efficiency packed columns, the HPLC-FLD parameter should be carefully investigated. In this work the performance of chromatography column packed with 2.6 μm core-shell particles on conventional benchmark HPLC were investigated. Parameters including flow rate, mobile phase composition (volume fraction of ACN in water), temperature, response time, sampling frequency, and injection volume for quantitative analysis of OTA in red wines were investigated in detail. The results show that core-shell column is more effective and faster to be operated on conventional HPLC than other total porous particle packed column. Optimized conditions provided a method for the separation of OTA in less than 5 min, with the limit of detection (LOD) 0.0025 μg/L and the limit of quantification (LOQ) 0.0083 μg/L in the sample, respectively. The developed method was validated with red wine samples with OTA concentrations ranging from 0.0028 to 0.0437 μg/L. The use of a core-shell column allows highly efficient, sensitive, and accurate determination of OTA with an outstanding sample throughout. © 2013 Elsevier Ltd.