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Development of a Dispersive Liquid–Liquid Microextraction Method for the Determination of α-Tocopherol in Pigmented Wheat by High-Performance Liquid Chromatography

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Abstract

A dispersive liquid–liquid microextraction (DLLME) method coupled to high-performance liquid chromatography was developed for the analysis of α-tocopherol in grain samples. The DLLME parameters including the type and volume of extractants, the volume of disperser and the addition of salt were examined. The optimized DLLME procedure consisted in the formation of a cloudy solution promoted by the fast addition to the sample (5 mL of saponified sample solution diluted with 5 mL of water) of a mixture of carbon tetrachloride (extraction solvent, 80 μL) and ethanol (dispersive solvent, 200 μL) without the addition of salt, followed by shaking for 5 min and centrifuging for 3 min at 5,000 rpm. Intra- and inter-day repeatability expressed as % RSD were 3.5 and 7.6 %, respectively. The limit of detection and the limit of quantification were 1.9 and 6.3 μg L−1. The comparison of this method with the national standardized extraction method, supercritical carbon dioxide extraction, accelerated solvent extraction, and conventional heat-reflux extraction indicates that the DLLME was accurate (no significant differences at the 0.05 % probability level), high efficient, low organic solvent-consuming, and low cost. This procedure was successfully applied to 42 samples of 14 types of purple wheat, for which the content of α-tocopherol exhibited a significantly negative correlation with the pigment content measured by a spectrophotometer. The recovery rates ranged from 90.5 to 103.7 %.

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Acknowledgments

The authors acknowledge with gratitude and appreciation financial support from Northwest A&F University.

Conflict of Interest

Qilong Xie declares that he has no conflict of interest. Shuhui Liu declares that she has no conflict of interest. Yingying Fan declares that she has no conflict of interest. Xiaoke Zhang declares that he has no conflict of interest. This article does not contain any studies with human or animal subjects.

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Authors and Affiliations

  1. College of Science, Northwest A&F University, No. 3 Taicheng Road, Yangling, Xianyang, Shaanxi, 712100, China

    Qilong Xie, Shuhui Liu & Yingying Fan

  2. State Key Laboratory of Crop Stress Biology in Arid Areas, Yangling, Xianyang, China

    Shuhui Liu

  3. College of Agronomy, Northwest A&F University, Yangling, Xianyang, China

    Xiaoke Zhang

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  1. Qilong Xie
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  2. Shuhui Liu
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  3. Yingying Fan
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  4. Xiaoke Zhang
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Correspondence to Shuhui Liu.

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Xie, Q., Liu, S., Fan, Y. et al. Development of a Dispersive Liquid–Liquid Microextraction Method for the Determination of α-Tocopherol in Pigmented Wheat by High-Performance Liquid Chromatography. Food Anal. Methods 7, 21–30 (2014). https://doi.org/10.1007/s12161-013-9592-x

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