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Fig 1.

Diagram of the UAE system.

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Table 1.

Variables and experimental design levels for RSM.

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Fig 2.

Effects of different extraction parameters (ethanol concentration, %; ultrasonic intensity, W/cm2; particle diameter, mm; extraction temperature, °C; ultrasonic time, min; solid-liquid ratio, mg/mL and extraction cycle) on yield of total phenolics from the T. chebula fruits.

Values were expressed as mean ± SD (n = 3), and evaluated by one-way AVONA followed by the Tukey test. Different letter and same letter were considered to be statistically significant (p < 0.05) and statistically insignificant (p > 0.05), respectively.

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Fig 2 Expand

Table 2.

The Box-Behnken experimental design with four independent variables.

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Table 2 Expand

Table 3.

ANOVA for response surface quadratic model analysis of variance table.

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Table 3 Expand

Fig 3.

Response surface (3D) and contour plots (2D) showing the effects of different extraction parameters (X1: ethanol concentration, %; X2: ultrasonic intensity, W/cm2; X3: solid-liquid ratio, mg/mL) added on the response Y.

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Table 4.

Predicted and experimental values of the responses at optimum conditions.

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Fig 4.

Antioxidant activities of the UAE extract, the CRE extract and Ascorbic acid.

(A) Reducing power, (B) FRAP, (C) DPPH radical-scavenging activity, (D) ABTS radical-scavenging activity and (E) superoxide radical-scavenging activity. Values were expressed as mean ± SD (n = 3), and evaluated by one-way AVONA followed by the Tukey test. Different letter and same letter were considered to be statistically significant (p < 0.05) and statistically insignificant (p > 0.05), respectively.

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Fig 5.

The HPLC chromatogram (a), total ion chromatogram of mass spectrometer in negative ion mode (b) and positive ion mode (c) of the T. chebula fruits extract.

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Fig 6.

The MS spectra in negative mode of seven representative compounds in the T. chebula fruits extract: shikimic acid (a), gallic acid (b), 5-O-galloylshikimic acid (c), corilagin (d), peak (e), 3,4,8,9,10-Pentahydroxydibenzo [b, d] pyran-6-one (f), ellagic acid (g).

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Fig 7.

The MS spectra in postitive mode of seven representative compounds in the T. chebula fruits extract: gallic acid (a), 5-O-galloylshikimic acid (b), corilagin (c), 3,4,8,9,10-Pentahydroxydibenzo [b, d] pyran-6-one (d), ellagic acid (e).

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Fig 7 Expand

Table 5.

HPLC-ESI-MS fragmentation (negative and positive ion mode) of the compounds detected in T. chebula fruit extract.

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Table 5 Expand