Plant collection and extraction
P. oleracea was collected from Sabzevar city, Khorasan Razavi province, Iran, in July 2017. A voucher sample was kept at the herbarium of the School of Pharmacy, Mashhad University of Medical Sciences (Herbarium No. 240-1615-12). The leaves of
P. oleracea were grounded to powder (100 g), mixed with 70% ethanol at a ratio of 1:10 (powder: ethanol) and left for 3 days at 37 °C with occasional shaking and stirring. The mixture was then filtered and the resulting liquid was concentrated under reduced pressure at 45 °C in an Eyela rotary evaporator (Heidolph, Germany). The yield of extraction was 17.5% (
9).
Animals
Experiments were performed using Wistar rats (200 ± 20 g) purchased from the animal house of School of Medicine, Mashhad University of Medical Sciences, Mashhad, Iran. The animals were kept in cages receiving clean filtered air (Maximiser, Thoren Caging System Inc., Hazleton, PA, U.S.A.) under standard conditions at 22 ± 2 oC with regular 12 hr/ 12 hr light/dark cycles. They also had free access to food and water ad libitum during the experimental period.
Animals sensitization
A rat model of asthma was induced by three i.p. injections of 1 mg/kg of OVA, along with 0.9% sterile saline containing 100 mg Al(OH)
3 as an adjuvant on days 1, 2 and 3 of the experiment. On days 6, 9, 12, 15, 18 and 21 of the experiment, animals were challenged with 1% OVA aerosol produced by a DeVilbiss PulmoSonic nebulizer (DeVilbiss Health Care Ltd., Feltham, U.K.) in a whole-body inhalation exposure chamber of 0.8 m
3 for 20 min/day (
16).
Experimental groups
Animals were randomly divided into six groups (n = 8 in each group) including: 1) Control group (group C) which was given intra-peritoneal (i.p.) and inhaled normal saline; 2) Asthmatic group (group A) which was sensitized with OVA; 3) Asthmatic group treated with dexamethasone 1.25 μg/mL (group A+D); and 4-6) Asthmatic groups treated with P. oleracea extract 1, 2, and 4 mg/mL (groups A+PO 1, 2, and 4 mg/mL, respectively). P. oleracea extract and dexamethasone were added to animals’ drinking water during the 21-day sensitization period. Each animal consumed almost 40 ml water per day and the volume of consumption was not significantly different among different groups; thus, dexamethasone-treated rats received 50 μg/day and PO-treated rats received 40, 80 or 160 mg/day of the extract for 21 days.
Collection of bronchoalveolar lavage fluid (BALF)
All rats were sacrificed on day 22 by ketamine (50 mg/kg, i.p.), their chest was opened, and the trachea and lungs were removed. The left lung was lavaged five times with 1 mL saline (a total of 5 mL). Then, BALF was centrifuged at 2500 g at 4 °C for 10 min and supernatants were collected and stored at -80 °C until analysis. Total and differential WBC counts as well as oxidant/anti-oxidant biomarkers levels were then assessed in the BALF.
Measurement of total and differential WBC count
To count total leukocytes, 1 mL of BALF was stained with Turk’s solution (containing 1 mL glacial acetic acid, 1 mL gentian violet solution 1% and 100 ml pure water) and total WBC was determined in duplicate using a hemocytometer (in a Burker chamber). The rest of BALF was centrifuged at 2500 g at 4 °C for 10 min. For differential WBC count, a smear was prepared from the cell pellet in BALF and stained with Wright-Giemsa. After staining, differential counts were determined in accordance with standard morphologic protocols under a light microscope by counting a total of 100 cells/slide. Then, the percentage of each leukocyte was calculated (
20).
Measurement of oxidant and antioxidant levels
Total stable oxidation products of NO metabolism (NO
2-/NO
3-) in BALF supernatant was evaluated using the Griess reagent containing sulfanilamide (SULF) and N-(1-Naphthyl) ethylenediamine dihydrochloride (NEDD). The frozen BALF was thawed at 25˚ C, and deproteinized using zinc sulfate (Sigma, America). The liquefied BALF was then centrifuged at 12000 g for 10 min. Next, 300 μL of the clear supernatant was mixed with Griess reagent in water, in a test tube. For reduction of nitrate to nitrite, 300 μL saturated solutions of vanadium (III) chloride (VCl
3; Sigma, USA) in 1 M HCl was added to the mixture and incubated for 2 hr at 30 °C, in the dark. Then, the absorbance of samples was assessed at 540 nm against a blank containing the same concentrations of ingredients but no biological sample. Linear regression was used to determine NO concentration using a standard curve plotted for NaNO
2. The final results were expressed as μmol (
20).
Moreover, MDA levels, as an index of lipid peroxidation, was measured. MDA reacts with thiobarbituric acid (TBA) as a thiobarbituric acid reactive substance (TBARS) to produce a red complex with the maximum absorbance at 535 nm. For MDA measurement, 2 mL of TBA/trichloroacetic acid (TCA)/HCl was added to 1 mL of BALF supernatant and the mixture was heated in a water bath for 40 min. Then, the mixture was centrifuged at 1000 g for 10 min. Finally, the absorbance was measured at 535 nm (
20).
A colorimetric assay involving production of superoxide by pyrogallol autoxidation and prevention of diminution of the tetrazolium dye, MTT (3-(4,5-dimethylthiazol-2-yl)2,5-diphenyltetrazolium bromide) to formazan by SOD, was used and measured at 570 nm (20). One unit of SOD activity was defined as the quantity of enzyme required for prevention of MTT reduction rate by 50%.
Catalase (CAT) activity was assessed based on the rate constant
k (dimension: S-1, k) of hydrogen peroxide decomposition. The reduction in absorbance at 240 nm per minute and the rate constant of the enzyme were determined. Activities were defined as k (rate constant) per liter (
20).
Total thiol concentration was measured using DTNB reagent which reacts with thiol moieties to produce a yellow complex with the maximum absorbance at 412 nm. Briefly, 1 mL tris-ethylenediaminetetraacetic acid (Tris-EDTA) buffer (pH 8.6) was added to 50 μL serum supernatant in 1-mL cuvettes and sample absorbance was read at 412 nm against Tris-EDTA buffer alone (A
1). Then, 20 μL DTNB reagents (10 mmol/ L in methanol) was added to the mixture and after 15 min (at room temperature), the sample absorbance was read again (A
2). The absorbance of DTNB reagent alone was also read as blank (B). Total thiol concentration (mmol/L) was calculated using the following equation (
20):
Total thiol concentration (mmol/L) = (A2–A1–B)×1.07/0.05×13.6.
Pathological evaluations
After sacrificing the animals, lungs were removed and placed into buffered formalin 10% (Merck, Darmstadt, Germany). Seven days later, tissues were dried using Auto Technicon apparatus and cleared by passage of tissues through 70–100% ethanol and xylol and paraffin blocks were prepared. The specimens were cut into 4-μm slices and stained with hematoxylin and eosin (H&E). The tissues were then evaluated under a light microscope. In this study, we focused on the following pathological changes in the lungs of asthmatic and treated groups: interstitial inflammation, interstitial fibrosis, bleeding, emphysema and epithelial damage. Scoring of pathological changes was performed as previously explained: 0) No pathologic changes; 1) Patchy changes; and 2) severe changes (in most parts of the lung) (
21).
Statistical Analysis
The data of total and differential WBC count, oxidant/antioxidant biomarkers levels and lung pathological studies were expressed as mean ± SEM. The comparisons of the data obtained from P. oleracea-treated groups, asthma group and control group were made using one way analysis of variance (ANOVA) with Tukey-Kramer’s post-test. Significance was accepted at p < 0.05.
Total WBC number (count/ml bronchoalveolar lavage fluid (BALF)), (a), percentages of eosinophils (b) and neutrophils (c) in control animals (C), asthma group (A), asthmatic rats treated with dexamethasone (A+D) and asthmatic rats treated with P. oleracea (PO 1, 2 and 4 mg/mL) (n=8 in each group). Data are presented as mean ± SEM values. * p < 0.05 and *** p < 0.001 show significant differences compared to group C. +++ p < 0.001 shows significant differences compared to group A. # p < 0.05, ## p < 0.01 and ### p < 0.001 show significant differences compared to group A+D. xxx p < 0.001 shows significant differences among the three concentrations of P. oleracea. Statistical analyses were performed using one way analysis of variance (ANOVA) with Tukey-Kramer’s post-test
Percentages of lymphocyte (a) and monocyte (b) in bronchoalveolar lavage fluid (BALF) of control animals (C), asthma group (A), asthmatic rats treated with dexamethasone (A+D) and asthmatic rats treated with P. oleracea (PO 1, 2 and 4 mg/mL) (n = 8 in each group). Data are presented as expressed as mean ± SEM values. * p < 0.05, ** p < 0.01 and *** p < 0.001 show significant differences compared to group C. + p < 0.05, ++ p < 0.01 and +++ p < 0.001 show significant differences compared to group A. ## p < 0.05, ## p < 0.01 and ### p < 0.001 show significant differences compared to group A+D. xx p < 0.01 and xxx p < 0.001 show significant differences among the three concentrations of P. oleracea. Statistical analyses were performed using one way analysis of variance (ANOVA) with Tukey-Kramer’s post-test
NO2 (a), NO3 (b) and MDA (c) concentration in bronchoalveolar lavage fluid (BALF) of control (C) asthma group (A), asthmatic rats treated with dexamethasone (A+D) and asthmatic rats treated with P. oleracea (PO 1, 2 and 4 mg/mL) (n = 8 in each group). Data are expressed as mean ± SEM values. ** p < 0.01 and *** p < 0.001 show significant differences compared to group C. +++ p < 0.001 shows significant differences compared to group A. # p < 0.05 and ### p < 0.001 show significant differences compared to group A+D. xx p < 0.01 and xxx p < 0.001 show significant differences among the three concentrations of P. oleracea. Statistical analyses were performed using ANOVA with Tukey-Kramer’s post-test
SOD (a), CAT (b) and Thiol (c) levels in bronchoalveolar lavage fluid (BALF) of control (C), asthma (A), asthmatic rats treated with dexamethasone (A+D) and asthmatic rats treated with P. oleracea (PO 1, 2 and 4 mg/mL) (n = 8 in each group). Data are expressed as mean ± SEM values. *** p < 0.001 shows significant differences compared to group C. + p < 0.05, ++ p < 0.01 and +++ p < 0.001 show significant differences compared to group A. ## p < 0.01 and ### p < 0.001 show significant differences compared to group A+D. xxx p<0.001 shows significant differences among the three concentrations P. oleracea. Statistical analyses were performed using ANOVA with Tukey-Kramer’s post-test
Interstitial inflammation (a), interstitial fibrosis (b) and bleeding (c) scores in control (C), asthma (A), asthmatic rats treated with dexamethasone (A+D) and asthmatic rats treated with P. oleracea (PO 1, 2 and 4 mg/mL) (n = 8 in each group). Data are expressed as mean ± SEM values. ** p < 0.01 and *** p < 0.001 show significant differences compared to group C. + p < 0.05, ++ p < 0.01 and +++ p < 0.001 show significant differences compared to group A. Statistical analyses were performed using ANOVA with Tukey-Kramer’s post-test
Emphysema (a) and epithelial damage (b) scores in control (C), asthma (A), asthmatic rats treated with dexamethasone (A+D) and asthmatic rats treated with P. oleracea (PO 1, 2 and 4 mg/mL) (n = 8 in each group). Data are expressed as mean ± SEM values. * p < 0.05, ** p < 0.01 and *** p < 0.001 show significant differences compared to group C. ++ p < 0.05, ++ p < 0.01 and +++ p < 0.001 show significant differences compared to group A. xx p < 0.01 shows significant differences among the three concentrations P. oleracea. Statistical analyses were performed using ANOVA with Tukey-Kramer’s post-test
Pathological studies of lung specimens under a light microscope (X40), in control (C), asthmatic (A) group with interstitial inflammation (II), interstitial fibrosis (IF), bleeding (B) and emphysema (E), asthmatic rats treated with dexamethasone (A+D) and asthmatic rats treated with P. oleracea (PO 1, 2 and 4 mg/mL)