A New Method for Analysis of Phenolic Acids in the Soil Soil from Replanted Apple Orchards was Investigated

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1 2013,46(21): Scientia Agricultura Sinica doi: /j.issn ( 1 / ) μ A New Method for Analysis of Phenolic Acids in the Soil Soil from Replanted Apple Orchards was Investigated YIN Cheng-miao 1, WANG Gong-shuai 1, LI Yuan-yuan 2, CHE Jin-shui 3, SHEN Xiang 1, CHEN Xue-sen 1, MAO Zhi-quan 1, WU Shu-jing 1 ( 1 College of Horticulture Science and Engineering, Shandong Agricultural University/State Key Loratory of Crop Biology Taian , Shandong; 2 Qingdao Bright Moon Bluesea Bio-Tech Co, LTD, Qingdao , Shandong; 3 Thermo Fisher Scientific, Shanghai ) Abstract: Objective To estlish a new protocol based on the ASE-HPLC method, which could determine the content of phenolic acids in orchard soil rapidly and efficiently. Method Phlorizin was set as an sample for analysis, which is one of the characteristic phenolic acids in apple orchard soil. Accelerated solvent extraction (ASE) combined with high performance liquid chromatography (HPLC) was used to assess it. Specifically, the parameters of extraction solvent, extraction temperature, pressure and number of cycles were optimized, aiming at exploring the optimal conditions of ASE extraction for phenolic acids. Result The optimal conditions of ASE extraction for phenolic acids were as follows: Ethanol as extraction solvent initially, and methanol was the subsequent extraction solvent extraction temperature at 120, a pressure of 10.3 MPa, 2 cycles, every 5 min static time, 60% purge volume, and purge time for 90 s. Conclusion The process was more simple, and with good reproducibility and linearity, correlation coefficient up to 0.99, recovery efficiency between 83% and 98%, detection limit to the amount of μg ml -1. ASE-HPLC is an accurate and rapid new protocol to mensurate phenolic acids, which is an improved and practical method. Key words: replanted apple orchards; phenolic acids; accelerated solvent extraction; performance liquid chromatography CARS-28IRT1155 yinchengmiao@163.com Tel mzhiquan@sdau.edu.cn

2 [1] [2-3] [4] [5] [6] [3] 80% [7-9] [10-12] NaOH [13] [3] Hartley and Buchan [13] 1 mol L -1 NaOH 15 h ph HPLC [3] 100 g 200 ml 0.45 μm 34 1 ml 0.22 μm HPLC Haghi [14] HPLC 4 Podsedek [15] [16] [17-18] [19-20] ph HPLC ASE-HPLC ASE ml Dionex Ultimate 3000 Dionex DGP-3600 WPS-3000TSL TCC-3000 DAD-3000 UV Milli-Q 18.2 MΩ cm 0.45 μm Sigma cm kg 12

3 mg kg mg kg mg kg mg kg g kg g 100 ml 1 ASE MPa 5 min 2 60% 90 s 34 1 ml 0.22 μm HPLC [3] g 250 ml 200 ml 34 1 ml 0.22 μm HPLC Acclaim 120 C18 3 μm 150 mm 3 mm 30 Dionex A B ph ml min -1 5 L 280 nm Microsoft Excel 2003 SPSS Extraction amount of Phlorizin (mg kg -1 ) Duncan s 0.05 Duncan's new multiple range test, Values followed by different letters in a figure are significant at the 5% level. The same as follows Fig. 1 Effect of different extraction solvents to extract phlorizin e d c a Extraction temperature ( ) Fig. 2 Comparison of extraction of different extraction temperatures

4 min 4 4 HPLC % 2 3.7% % 2 5.0% % 95.5% 2 ph ph ml min -1 5 μl A B 0 35 min 5% 35% min 35% min 35% Extraction amount of Phlorizin (mg kg -1 ) Fig. 3 Comparison of extraction rate of different extraction cycles 5% 10 min 10 mg 10 ml 10 ml 30 μg ml μg ml -1 HPLC S/N=3 4 1 mau Gallic acid; 2. P-hydroxybenzoic acid; 3. Catechin; 4. Caffeic acid; 5. Syringic acid; 6. Vanillic aldehyde; 7. Ferulic acid; 8. Phloroglucinol; 9. Benzoic acid; 10. Salicylic acid; 11. Phlorizin; 12. Quercetin; 13. Cinnamic acid; 14. Phloretin Fig. 4 The phenolic standard measurement spectrum of 14 kinds of phenolic acids

5 Tle 1 Retention time, linear equation, correlation coefficient and detection limit R 2 Number Phenolic Compound Retention time (min) Linear equation Correlation coefficient Detection limit (μg ml -1 ) 1 Gallic acid 2.95 y=2.652x P-hydroxybenzoic acid y=1.1476x Catechin y=0.5233x Caffeic acid y=6.4564x Syringic acid y=14.453x Vanillic aldehyde y=8.9167x Ferulic acid y=3.1315x Phloroglucinol y=0.5513x Benzoic acid y=0.2194x Salicylic acid y=0.2223x Phlorizin y=3.3742x Quercetin y=0.5518x Cinnamic acid y=6.4602x Phloretin y=4.4998x B mg Tle 2 Determination results of apple replanted orchard soil and recovery test Number Phenolic compound A Count B Count Recovery % RSD (mg kg -1 ) (mg kg -1 ) 0.25 mg kg mg kg mg kg -1 (% n=5) 1 Gallic acid 0.005g ND P-hydroxybenzoic acid 0.066f ND Catechin 0.047fg 0.021b Caffeic acid 0.068f ND Syringic acid 0.041fg ND Vanillic aldehyde 2.208a 0.031a Ferulic acid 0.065f ND Phloroglucinol 0.055fg ND Benzoic acid 0.036fg 0.015c Salicylic acid 1.859b ND Phlorizin 0.212e ND Quercetin ND ND Cinnamic acid 0.273d ND Phloretin 0.489c ND ND A B ND: not detected, A: ASE extraction method, B: Organic solvent extraction method

6 A mg kg % 98% 5 RSD Hartley Buchan [13] 1 mol L -1 NaOH ph HPLC [21] NaOH [21] [3] 12 h 200 ml 25 min ASE-HPLC [22-25] [26-28] HPLC ph [29] 12 HPLC Hilt [30] HPLC MS NMR Schieber [31] 60 min [3] 42 min 10 HPLC [3] ph ph HPLC MPa 2 5 min 60% 90 s HPLC ph ml min -1 5 μl A B 0 35 min 5% 35% min 35% min 35% 5% 10 min 83% 98%

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