Eco-friendly extraction and simultaneous determination of two coumarins in <i>Justicia pectoralis</i> (Acanthaceae)

Lima, Alessandra Ribeiro Sartor; Lôbo, Luan Augusto Cândido; Costa, Thaísa Lorrana da Cruz; Peixoto, Josana de Castro; Borges, Leonardo Luiz; Amaral, Vanessa Cristiane de Santana; Paula, Joelma Abadia Marciano de

doi:10.1590/2175-7860202071041

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Pharmacognosy • Rodriguésia 71 • 2020 • https://doi.org/10.1590/2175-7860202071041 copy

Eco-friendly extraction and simultaneous determination of two coumarins in Justicia pectoralis (Acanthaceae)

Authorship SCIMAGO INSTITUTIONS RANKINGS

Abstract

Justicia pectoralis (Acanthaceae) is employed in folk medicine for its analgesic, anti-inflammatory and sedative effects and to treat respiratory diseases. It is known for properties of its coumarins, 1,2-benzopyrone and umbelliferone. A green, simple, fast, and inexpensive ultrasound-assisted extractive (UAE) method for extracting umbelliferone and 1,2-benzopyrone from Justicia pectoralis was optimized. Additionally, a HPLC analytical method was developed and validated for the simultaneous determination of both coumarins. The Box-Behnken design and response surface methodology were used to evaluate the UAE process. Ethanol concentration, extraction time, plant-to-solvent ratio were the independent variables studied and the coumarin content was the dependent one. The HPLC-UV/VIS method was validated in terms of recovery, linearity, accuracy, precision and robustness, proving to be valuable for the quality control of Justicia pectoralis extract and in the development of its herbal products. Results show that the optimal UAE conditions were: ethanol concentration of 15% (w/w), extraction time of 34 min and plant-to-solvent ratio of 0.1 g/mL. The predicted values of coumarin contents (22.16 µg/mL - umbelliferone and 163.86 µg/mL - benzopyrone) were determined under the optimal UAE conditions and proved that UAE is an efficient and eco-friendly extractive process for the production of aerial part extracts from Justicia pectoralis.

Key words:
benzopyrone; Box-Behnken design; response surface methodology; umbelliferone

System suitability
	Tailing factor (TF)	Resolution (Rs)	Theoretical plates (N)
Sample umbelliferone peak	0	2.97 (± 0.05)	5157.8 (± 259.37)
Sample 1,2-benzopyrone peak	1.03 (± 0.01)	2.16 (± 0.05)	6220 (± 241.65)
Literature recommendations (ICH 2005)	≤ 2.00	≥ 2.00	> 2000.00

	Umbelliferone	1,2-Benzopyrone
Linear range (µg/mL) Limit of detection (µg/mL) Limit of quantification (µg/mL)	29.7 - 2.4 0.3539 1.1799	512.0 - 41.3 5.8110 19.3700
*Linear regression data^ * y = ax + b, where x is the compound concentration and y is the peak area.**
N	6	6
Slope (a) Standard deviation of slope	36778 210.01	22473 125.19
Relative standard deviation of slope (%)	0.57	0.55
y-axis intercept (b)	14097	133760
Linear correlation coefficient (r)	1.0000	1.0000

Coumarins	% Assay (Day-1, Analyst-1)	% RSD of Assay (N = 6)	% Assay (Day-2, Analyst-2)	% RSD of Assay (N = 6)	% RSD Inter -day
1,2-Benzopyrone	0.778	2.77	0.732	5.91	5.35
Umbelliferone	0.096	3.61	0.087	4.65	6.55

Coumarins	Levels (%)	Amount recovered (mg/mL)	% Recovery	Mean % recovery	% RSD
1,2-Benzopyrone	Low	16.00	95.46
	Medium	20.00	95.70	94.07	3.65
	High	24.00	91.06
Umbelliferone	Low	16.00	99.30
	Medium	20.00	95.57	94.93	4.81
	High	24.00	89.92

Run number	X₁ (%)	X₂ (min)	X₃ (g/mL)	Umbelliferone (µg/mL)	1,2-Benzopyrone (µg/mL)
1	15	20	0.07	14.00	166.78
2	45	20	0.07	10.41	105.63
3	15	60	0.07	16.81	109.34
4	45	60	0.07	12.34	118.24
5	15	40	0.10	22.58	161.04
6	45	40	0.10	17.95	171.47
7	15	40	0.05	11.41	84.85
8	45	40	0.05	9.81	86.46
9	30	20	0.10	17.38	150.69
10	30	60	0.10	21.62	163.11
11	30	20	0.05	7.81	71.51
12	30	60	0.05	9.94	85.52
13	30	40	0.07	12.34	111.61
14	30	40	0.07	12.59	110.67
15	30	40	0.07	12.47	106.48

Factor	Sum of squares	Degrees of freedom	Mean squares	F value	p
X₁	24.9761	1	24.9761	1597.62	0.000625^* * p < 0.05.
X₂	12.5611	1	12.5611	803.48	0.001242^* * p < 0.05.
X₃	179.2208	1	179.2208	11464.02	0.000087^* * p < 0.05.
X₁²	3.1250	1	3.1250	199.89	0.004965^* * p < 0.05.
X₃²	2.1819	1	2.1819	139.57	0.007089^* * p < 0.05.
X₁ X₂²	0.4186	1	0.4186	26.78	0.035376^* * p < 0.05.
X₁²x₂	0.3321	1	0.3321	21.24	0.043990^* * p < 0.05.
X₁²X₂²	0.0985	1	0.0985	6.30	0.128760
X₁X₃	2.2952	1	2.2952	146.82	0.006742^* * p < 0.05.
X₁²X₃	0.4705	1	0.4705	30.09	0.031661^* * p < 0.05.
X₂X₃	1.1130	1	1.1130	71.20	0.013757^* * p < 0.05.
Lack-of-fit	0.193	1	0.1936	12.38	0.072124^* * p < 0.05.
Pure error	0.031	2	0.0156
Sum of squares total	268.3766	14

Factor	Sum of squares	Degrees of freedom	Mean squares	F value	p
X₁	39.68	1	39.68	5.319	0.147508
X₁²	1.65	1	1.65	0.221	0.684861
X₂	3.22	1	3.22	0.432	0.578452
X₃	11268.90	1	11268.90	1510.692	0.000661^* * p < 0.05.
X₁ X₂	1226.75	1	1226.75	164.456	0.006026^* * p < 0.05.
X₁X₃²	516.65	1	516.65	69.261	0.014133^* * p < 0.05.
X₁²X₃²	1.83	1	1.83	0.246	0.669163
X₂X₃²	634.75	1	634.75	85.093	0.011549^* * p < 0.05.
X₂²X₃	2.45	1	2.45	0.329	0.624220
X₂²X₃²	38.99	1	38.99	5.227	0.149562
Lack-of-fit	20.08	2	10.04	1.346	0.426266
Pure error	14.92	2	7.46
Sum of squares total	15885.45	14

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[1] 3Author for correspondence: joelma.paula@ueg.br

	DF	SS	MS	F	F tab
Umbelliferone	1	2.27107E+12	2.27107E+12	30942.13704	7.65878E-22
Residual	16	1026008626	64125539.1
Lack-of- Fit	4	145239380.3	36309845.07	0.494701811	0.74009069
Pure error	12	880769245.3	73397437.11
	DF	SS	MS	F	*F tab*
1,2-Benzopyrone	1	2.52336E+14	2.52336E+14	221259.0286	5.73934E-27
Residual	16	28011982530	1750748908
Lack-of- Fit	4	14326544369	3581636092	3.140537599	0.055327445
Pure error	12	13685438161	1140453180