Determination of 1, 9-Decanediol in Soil with Ultrasonic Extraction-Gas Chromatography
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S145.9

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Supported by the NSFC-JST Project (No. 31761143015),the Natural Science Foundation for Distinguished Young Scholar of Jiangsu Province of China (No. BK20190108)and the Key Research and Development Program of Shandong Province of China (No. 2019JZZY010701)

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    Abstract:

    [Objective] The application of biological nitrification inhibitors (BNIs) is considered an important new strategy to reduce nitrogen loss from agricultural systems. Recently, a new BNI, 1,9-decanediol, has been identified in rice root exudates and the substance is found to be contributive to improvement of nitrogen (N)-use efficiency (NUE) and reduction of N2O emissions in agriculture. In order to evaluate its stability and effect in soil, an efficient, fast and accurate extraction and detection method needs to be developed. Thus, this study was oriented to develop a method of using ultrasonic extraction-gas chromatography (GC) to determine 1,9-decanediol in soil.[Method] Soil samples were collected from a paddy soil at Yixing (31°17' N, 119°54' E), Jiangsu Province of China for extraction of 1,9-decanediol using different methods, including different extractants (water, acetonitrile, methanol, acetone, ethyl acetate, dichloromethane, hexane, and petroleum ether), different liquid to solid ratios (varying in the range of 10-50 mL·g-1), different durations of ultrasonic processing (in the range of 10-50 min), different frequency of extraction (in the range of 1-3 times), and different gas chromatography detection parameters, including inlet temperature (in the range of 200-280℃), detector temperature(in the range of 260-320℃), and four heating procedures for optimization. Spike recovery of the substance in soil was determination relative to its concentration (10, 100 and 1 000 mg kg-1).[Result] Results show that:(1) the method of ultrasonic extraction using methanol as extractant, 40 mL·g-1 in liquid/solid ratio, and going only one round that lasted 30 min was the optimal one; (2) In using the Agilent 8890 gas chromatographer to determine the substance, the optimal conditions were 250 ℃ at the inlet, 310 ℃ at the FID detector, 60 ℃ in the column kept for the first 2 min, and then raised up to 150 ℃ at 20 ℃·min-1 and to 180℃ at 3℃·min-1, kept for 2 min. and in the end, raised to 270 ℃ at 20℃·min-1; (3) under such conditions, determination of 1,9-decanediol, 10-100.00 μg·mL-1 in concentration exhibited good linearity, standard curve of y=26.81x-9.678(R2=0.999), detection limit of 0.03 μg·mL-1, recovery rate of 93.99%-96.91%, intraday precision 1.78% and interday precision of 1.52%; and (4) under such optimal extraction and determination conditions, the spike recovery rate of 1, 9-decanediol in soil samples, regardless of concentration, varied in the range of 90.58%-94.55% with relative standard deviation(RSD)varying in the range of 0.30%-3.41%.[Conclusion] This method, low in detection limit, high in sensitivity and precision, and good in reproducibility, and this experiment may lay down a foundation for evaluation of stability and environmental impacts of 1, 9-decanediol in agricultural soils, and provide a good reference for developing methods for extracting other BNIs in soil in future.

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YANG Ting, LU Yufang, MA Mingkun, SHI Weiming. Determination of 1, 9-Decanediol in Soil with Ultrasonic Extraction-Gas Chromatography[J]. Acta Pedologica Sinica,2021,58(4):968-977.

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History
  • Received:November 21,2019
  • Revised:March 09,2020
  • Adopted:May 08,2020
  • Online: December 10,2020
  • Published: July 11,2021