Extraction of Pectin from Lemon Peel and its use as a Natural Binder in Aspirin Tablet

Prajakta M. Patil^*, Omprasad S. Nayakal, Mangesh Bhutkar, Somnath Bhinge, Dheeraj Randive

Rajarambapu College of Pharmacy, Kasegaon, Tal- Walwa. Dis- Sangli Maharashtra -India 415404

*Corresponding Author E-mail: prajaktap392@gmail.com

ABSTRACT:

Lemon peels after removing the lemon juice are generally discarded. The potential of this waste material was explored in the present research work. The study aimed to extract pectin from the dried lemon peels and to assess its utility as a natural binder in tablets using Aspirin as a model drug. Pectin was extracted under pH 2; Ethanol ratios(ER) 1:1 and extraction periods 120 min, at this condition highest yield of 18.21% was obtained. Citrus peels were previously treated with ethanol, and the obtained alcohol insoluble solids (AIS) were subjected to a sequential extraction. The method of extraction was Soxhlet distillation. After successful extraction and isolation of pectin from the dried lemon peels, it was investigated for its binding property in tablet. The binding property of isolated pectin was compared with HPMC. Pre-compression and post-compression evaluation studies were performed for all the prepared formulations and found to be within the range as prescribed in the pharmacopoeias. In vitro dissolution studies revealed that Batch F3 showed 62.66 % drug release, whereas Batch F6 which comprised of HPMC as a binder exhibited highest drug release of 90.30% amongst all the formulations used in the study. The results of the study thus, revealed that pectin from lemon peel can act as excellent binder in dosage forms. Since, it is of natural origin and lemon peels are usually available at low cost it may prove to be a better binder as compared to commercially used synthetic binders.

KEYWORDS: Pectin, HPMC, Aspirin, Drug release.

INTRODUCTION:

Pectin is a purified carbohydrate product obtained from the inner portion of lemon peel. Pectin mostly consists of polygalacturonic acid.¹It is produced in the form of white to light brown powder. It mainly extracted from citrus fruits and mostly used in food as a gelling agent particularly in jams and jellies.²

It is a polysaccharide consisting of two moieties. These are homogalacturonan, (1-4) linked, a-Dgalacturonic acid and its methyl ester.

Pectins have been used in food industry but recently they are being explored for their other pharmaceutical applications such as binding, thickening, suspending properties. For this study, Aspirin was selected as a model drug, which is analgesic and inflammatory in nature.³

The scope of the present work was to assess the utility of pectin from lemon peel as a binding agent, against the commercially used one’s like HPMC.⁴

MATERIALS AND METHOD:

Materials:

Pure drug was procured from the Research Scientific, Mumbai. All other chemicals and reagents used were of analytical grade. Fresh lemon fruit was purchased from local market. It was cut into pieces and squeezed to remove all the juice. The peels were then further cut into small pieces and shade dried.

Method:

1. Extraction:

Dried lemon fruit peel powder (200g) was used for extraction using Soxhlet apparatus. The water to be used for extraction was acidified using 0.5N citric acid and pH was maintained about 2. The content of the round bottom flask was heated continuously at 75º C for around 7 to 8 h after the start of first siphon cycle. The proportion of powder to solvent was taken in ratio 1:4. After the heating period was over, the mixture was passed through two fold muslin cloth and was cooled to room temperature.⁵

2. Isolation of pectin:

Isolation of pectin was carried out using ethyl alcohol as precipitating agent. Ethyl alcohol was used as a precipitating agent for pectin. For this purpose, twice amount of ethyl alcohol was added to the cooled solution and continuous stirring was done for 15 min. Then the mixture was kept aside for 2h without stirring. Pectin was filtered through four layered muslin cloth. The precipitate was washed 2 to 3 times by ethyl alcohol, to further remove any remaining impurity. Finally, precipitate was kept for drying at 35ºC to 40ºC in hot air oven, and percentage yield was found to be around 18.36%. It was then stored in desiccators until further use.⁶

Table No 1: Composition of Aspirin tablets prepared by direct compression

Ingredients (mg)	F1	F2	F3	F4	F5	F6
Aspirin	75	75	75	75	75	75
PVP	20	20	20	20	20	20
Pectin	10	20	30	-	-	-
HPMC	-	-	-	2	3	4
Talc	6	6	6	6	6	6
Magnesium stearate	4	4	4	4	4	4
Microcrystalline cellulose	q.s	q.s	q.s	q.s	q.s	q.s
Total weight (mg)	200 mg	200 mg	200 mg	200 mg	200 mg	200 mg

3. Preparation of Tablet:

Six different batches of tablets were prepared using dry granulation technique. The composition of single tablet per batch is given in Table no 1. Tablets of 200mg were prepared by direct compression. All the ingredients are weighed accurately (Aspirin, Pectin, Starch, MCC, PVP, Magnesium stearate, and Talc) and triturated using mortar and pestle. These blends of powder were passed through 20 mesh sieve in order to remove foreign material and to get uniform particle size. The powder was blended in a poly bag by tumbling for five minutes. The blend was transferred directly into the hopper of single punch machine having caplet shaped concave punch and was compressed manually.

Pre-compression evaluation:^7-11

Evaluation of granules:

The prepared granules were evaluated for all pre-compression parameters like angle of repose, bulk density, tapped density, Hausner’s ratio and Carr’s index.

1. Angle of Repose:

It was determined using fixed funnel method. The blend was poured through a funnel that can be raised vertically until a maximum cone height (h) was obtained. Radius of the heap (r) was measured and angle of repose was calculated using formula:

θ= tan^-1(h/r)

2. Bulk density:

It is the ratio of total mass of powder to the bulk volume of powder. It was measured by pouring the weight powder (passed through standard sieve # 20) into a measuring cylinder and initial volume was noted. This initial volume is called the bulk volume. From this, the bulk density was calculated according to the formula mentioned below. It is expressed in g/ml and is given by:

Weight of granules

Bulk density= --------------------------------------------------------------

Volume occupied by granules

3. Tapped density:

It is the ratio of total mass of the powder to the tapped volume of the powder. Volume was measured by tapping the powder for 750 times and the tapped volume was noted. It is expressed in g/ml and is given by:

Weight of granules

Tapped density=----------------------------------- Volume occupied by granules

4. Hausner’s ratio:

It is an indirect index of ease of powder flow. It is calculated by the following formula:

HR = Tapped density

---------------------------------------------------------------

Bulk density

5. Carr’s compressibility index:

It is calculated by the following formula:

Tapped density - Bulk density

Compressibility =------------------------------------------------------------------ X 100

Tapped density

Post compression study:

1. Weight variation:

All prepared tablets were evaluated for weight variation as per USP XXIV monograph. Thirty six tablets of each batch were used to evaluate weight variation among tablets and mean and standard deviation was calculated.

2. Friability:

Tablets of all batches were used to evaluate friability as per USP XXIV monograph. Friability testing was done by BESTO Apparatus.

3. Hardness:

Hardness of all batches was determined using Tablet Hardness Tester Monsanto type. The test was carried out in triplicate for all batches as per USP XXIV monograph for uncoated tablets.

4. Disintegration test:

Disintegration test was carried out using disintegration rate test apparatus. Tablets were placed in the dissolution medium 0.1 N HCl.

5. In vitro dissolution study:

The release of drug from drug was determined using USP dissolution testing apparatus 2. The dissolution test was performed using 900 ml of phosphate buffer pH 6.8 at 37 ±0.5°C and 50 rpm. A sample (10 ml) of the solution was withdrawn from the dissolution apparatus at different time intervals and the samples were replaced with fresh dissolution medium. The samples were filtered through a 0.45μ membrane filter and diluted to suitable concentration with buffer pH 6.8. Absorbance of these solutions was measured at 222 nm using a UV/Vis spectrophotometer. Cumulative percentage drug release was calculated using an equation obtained from a standard curve.^12-18

RESULTS AND DISCUSSION:

As per the data obtained by the experiment, pectin derived from Lemon peels showed good binding property as compared to HPMC. The various micromeritic characteristics and flow properties of the granules obtained by dry granulation for each batch and reference batch did not show any significant variation in their values. The values of physical properties of all batches are shown in evaluation test table having average of triplicate readings, with standard deviation.

The prepared tablets were evaluated for post compression parameters such as weight variation, hardness, thickness, drug content uniformity, and in vitro release characteristics. The readings were obtained in triplicate and values were presented as mean with standard deviation. The pre-compression evaluation data is tabulated in Table no 2.

Table No 2: Pre-compression Evaluation Parameters

Batch code	Bulk density(gm/ml)	Tap density(gm/ml)	Angle of repose	Carr’s Index	Hausner’s Ratio
F1	0.39±0.04	0.49±0.02	25.7±1.24	14.54±0.59	1.765±0.162
F2	0.42±0.07	0.56±0.09	29.7±0.49	13.65±0.33	1.876±0.150
F3	0.46±0.11	0.59±0.02	21.45±0.65	13.87±0.07	1.654±0.164
F4	0.54±0.09	0.58±0.02	22.76±0.75	14.87±0.76	1.765±0.343
F5	0.50±0.07	0.62±0.11	26.65±0.37	13.1±0.65	1.765±0.343
F6	0.52±0.02	0.60±0.04	25.43±0.86	15.6±0.57	1.589±0.191

(Values are S.D+ n=3)

Table No 3: Post-compression study of the prepared tablets

Batch Code	Weight variation (mg)	% Friability	Hardness(Kg/cm²)	Disintegration time (sec)
F1	197.5±1.10	0.5689±0.01	2.5±0.21	86±0.11
F2	197.21±0.85	0.4691±0.03	3.1±0.32	56±0.17
F3	198.15±0.45	0.7806±0.03	3.0±0.32	87±0.09
F4	198.7±0.56	1.0037±0.09	2.7±0.094	69±0.18
F5	197.77±0.09	1.2562±0.14	2.7±0.04	90±0.12
F6	223.35±0.62	1.209±0.13	3.5±0.37	79±0.13

(Values are S.D + n=3)

Post compression evaluation:

The results of various post compression evaluation of tablets are shown in Table no 3.

In-vitro drug release study:

In-vitro drug release was studied using Lab India Dissolution Apparatus (LABINDIA DS 8000, India), in 900 ml phosphate buffer pH 6.8, maintained at 37±1°C for 3 h, at 50 rpm. 10ml of sample was withdrawn after specified time interval, and was replaced by an equal volume of fresh dissolution medium. Collected samples were analyzed spectrophotometerically at measured wavelength of 222nm, and cumulative percent drug release was calculated. Drug release profile was studied using percentage drug release Vs time (h) plot.

Table No.4. In vitro Cumulative % Drug Release

Time (min)	F1	F2	F3	F4	F5	F6
30	1.30±0.12	10.95±0.11	15.15±0.14	14.99±0.17	17.12±0.17	18.12±0.17
60	2.24±0.09	18.76±0.18	26.82±0.18	17.52±0.19	19.88±0.15	24.98±0.11
90	4.62±0.17	26.14±0.17	35.66±0.24	19.69±0.15	34.94±0.16	48.76±0.16
120	8.47±0.13	38.42±0.16	42.06±0.91	34.84±0.13	45.35±0.13	59.29±0.88
150	10.67±0.18	43.09±0.15	58.82±0.16	54.24±0.12	65.41±0.21	65.77±0.12
180	20.42±0.17	54.35±0.17	62.66±0.14	68.02±0.14	85.21±0.08	90.30±0.92

(Values are S.D + n=3)

Cumulative percentage drug release study:

Fig No 5: Drug release profile of Aspirin tablets

CONCLUSION:

Pectin from lemon peel as a binder produced tablet formulations with good hardness, friability, disintegration time and dissolution rate. Thus, on the basis of the above experimental results it can be concluded that lemon peel pectin which is polymer of natural origin has immense potential to replace commercially existing polymers used as binder in tablet formulation.

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Received on 05.04.2018 Accepted on 15.06.2018

Asian J. Pharm. Tech. 2018; 8 (3):115-118 .

DOI: 10.5958/2231-5713.2018.00018.1