INTRODUCTION:

Anthocephalus cadamba (Roxb.) (Family: Rubiaceae) is known as ‘‘Kadamba’’ in Sanskrit in India¹. It is traditional ayurvedic plant widely used in the treatment of various ailments like diabetes mellitus, cough, vomiting, wounds, leprosy, ulcers, stomatitis, dyspepsia, diarrhoea, fever, inflammation, cancer and also used for its diuretic, anthelmintic, hepatoprotective and antimicrobial activity^1,2,3,4,5. The major constituents of the plant are triterpenes, triterpenoid glycosides, flavanoids, saponins, indole alkaloids; cadambine, cadamine, isocadambine, isodihydrocadambine^1,2.

A decoction of the leaves was consumed for the treatment of ulcers and wounds since long, and it is prescribed for the treatment of elephantiasis in Bangladesh since ancient times². The Charaka Samhita describes the use of leaves for curing pimples and wounds². The leaf juice is also used for relieving burning sensation of palms and feet². The extract of the leaf is used as gargle for throat infection due to its astringent properties². The Sushruta Samhita describes the use of leaf as analgesic agent, and in the treatment of rheumatism and inflammation of glands². Ayurveda also describes the use of leaves in the treatment of obesity². Aqueous extract of Cadamba leaves shows antipyretic, antidiabetic, immunomodulatory and analgesic effect^{6,7, 8,9}. Aqueous and alcoholic extract of Cadamba leaves shows antibacterial, antifungal, wound healing anti-inflammatory and antioxidant activity^10,11,12. The methanolic extract of leaf of shows beneficial effects in reducing the elevated blood glucose level of hyperglycemic mice¹³. The extract of the leaves also shows cytotoxic activity against different human cancer cells¹⁴. Aqueous extract of leaves increases the level of haemoglobin, red blood cells and white blood cells and it reduced the levels of glucose, total cholesterol¹⁵. Taking into consideration these activities shown by this plant there is need to prepare formulation consisting of cadamba leaf extract.

Divyakant Patel etal developed and evaluated Herbal Syrup using extract of leaves of cadamba plant¹⁶. Liquid dosage forms have some limitations like possibility of active ingredients degradation in presence of water, requirement of more space, difficulty in transportation as it is liquid formulation. To overcome this limitations powder can be prepared from aqueous extract by spray drying process.

Spray drying is commonly used method for converting a wide range of liquid extracts into powder form. This process results in powders of good quality, low water activity and makes it easy for transport and storage. The physicochemical properties of powders produced by spray drying process depend on some process variables like flow rate of the liquid feed and drying air temperature. Powders obtained by spray drying shows problems like stickiness, hygroscopicity. When powders stick on the dryer chamber wall during drying, and which reduces % yield of product and also it can causes operational problems. Stickiness depends on temperature and moisture content. If amorphous powders are at temperatures and/or moisture contents higher then particles sticks with another particle¹⁷.

Therefore, it is important to use suitable spray drying agent like maltodextrin, glucose, soybean protein, aerosil. These are high molecular weight substances with high glass transition temperatures so it minimizes sticking. Besides reducing powder hygroscopicity, such agents, normally used for microencapsulation, can protect sensitive active ingredients against unfavorable ambient conditions, mask or preserve flavors and aromas and reduce the volatility and reactivity¹⁷.

Aerosil is used as spray drying agent for preparation of herbal extract obtained from different plants like Tanacetum parthenium¹⁸, Psidium guajava¹⁹, Mikania glomerata²⁰, Glycyrrhiza glabra²¹, Ilex paraguariensis²², Maytenus ilicifolia²³.

MATERIAL AND METHODS:

Collection of plant material, Chemicals and reagents:

The Anthocephalus cadamba leaves used were obtained from tree at Sangamner (Maharashtra State, India). Specimen containing leaves, fruits and flowering top of this plant was collected locally and sent for authentification. Authentification Report of plant was received from Botanical Survey of India, Pune. All other chemicals and reagents used were analytical grade.

Preparation of extract:

Anthocephalus cadamba leaves were shade dried, powdered. This powder was boiled with water (1part of powder with 10 part of water) to obtain extract. The extract was then filtered using Filter Paper and transferred to a bottle. Filtration was carried out to remove of fibers at room temperature. The extracts obtained were stored at refrigerator at 4°C for one day if required^{21, 24}.

Spray drying of cadamba extract using Aerosil as spray drying agent:

Above aqueous extract was subjected to spray drying using laboratory scale Labultima UV222 spray drier. Experimental conditions followed for optimization as per Table 1.

Table 1. Experimental conditions for spray drying of cadamba leaves extract using Aerosil as spray drying agent.

No. of Experiment	Drying aid (Aerosil) concentration (%)	Air inlet temperature (^○C)	Feed flow rate (mL/min)
1	6	110	2
2	6	125	1
3	6	125	3
4	6	140	2
5	8	110	1
6	8	110	3
7	8	125	2
8	8	140	1
9	8	140	3
10	10	110	2
11	10	125	1
12	10	125	3
13	10	140	2
14	10	140	1

Evaluation Parameter for Spray dried Powder:

Yield:

Yield of product after spray drying is calculated as the ratio between the total mass of recovered product and the mass of total solid initially fed into the system. Process yield was calculated as the relationship between total solids content in the resulting powder and total solids content in the feed mixture¹⁷.

Moisture content:

For determination of moisture content, 1g of each powder was placed in an oven dryer at 80°C for 3 hrs. Samples were cooled in dessicators for 1 hr and then weighed. Moisture content was determined as percentage mass loss¹⁷.

Time required for solubilization:

A small sample of dry powders of 0.6 g was added to 400 mL of water at 70 °C in a 500 mL beaker. The mixture was stirred using a magnetic stirrer at 100 rpm. Solubility was measured as the time in seconds to dissolve the dry powders completely²⁵.

Bulk density:

Bulk density was determined by adding 2 g of powder to a 10 mL graduated cylinder and holding the cylinder on a vibrator for 1 min. The bulk density was calculated by dividing mass of the powders by the volume occupied in the cylinder²⁵.

Hygroscopicity:

Samples (1 g) of each powder were placed in small glass covers, weighed and kept at relative humidity of 75 % in stability chambers at 25 °C. After seven days, the samples were weighed and the hygroscopicity is expressed as gm moisture/100 gm solids¹⁷.

RESULTS :

Interaction effects of the process variables on the efficiency of the spray drying process:

Interactions among spray drying process parameters, i.e., air inlet temperature, feed flow rate and % of drying aid obtained are summarized in Figure 1-6. Powder characteristics such as moisture content, bulk density were examined in this study to optimize the spray drying operating conditions. The highest efficiency of spray drying (65%) was achieved when the air inlet temperature was140°C. There were also significant effects of air inlet temperature and feed flow rate on the efficiency of spray drying process. The highest predicted efficiency of the spray drying 65% was found at air inlet temperature of 140 °C together with feed flow rate at 1mL/min. Therefore, these parameters are taken into consideration for the spray drying of cadamba aqueous extract to avoid problems like stickiness and deposition on the chamber wall. It was observed that there was not enough heat to dry the extract at low air inlet temperature, so some moisture remained in the dried product that resulted moist powder to stick on surface of the drying chamber and yield obtained was also low at low inlet temperature²⁶.

Yield:

As temperature increases % yield also increases. Highest yield is obtained at 140^○C inlet temperature and at 10% of aerosil as drying aid. (Table-2)

Moisture content:

Inlet air temperature and drying aids reduced the moisture content, which is desirable for the spray drying process. Generally, the greater the temperature differences between the particles and air surrounding it, the greater the evaporation rate. Moisture content also decreased with increasing concentration of drying aid. Least moisture content was observed at 140^○C inlet temperature, 10% of aerosil as drying aid and 1mL/min feed flow rate. (Table-2)

Bulk density:

The bulk density decreased with increasing inlet air temperature. The bulk density of powders was in the range 0.22 –0.42 gm/mL. At higher temperature of inlet air resulted in a rapid formation of vapour-impermeable film of dried layer at the droplet surface and the particle size was more at the higher temperatures. This effect decreased bulk density of powder. (Table-2)

Time required for solubilization:

Solubility was measured as the time in seconds to dissolve the dry powders completely and it was found in range of 30-56 seconds. (Table-2)

Hygroscopicity:

Hygroscopicity is expressed as quantity of moisture in gm absorbed per 100 gm solids in 7 days period. It is observed to be 25-67gm /100gm. Higher % of drying agent resulted in least hygroscopic powder because evaporation process was fast and product obtained was more porous or fragmented structure, and the particles were hollow²⁷. (Table-2)

Table 2. Properties of Anthocephalus cadamba extract powder.

No. of Experiment	Yield (%)	Moistur Content (%)	Bulk Density gm/mL	Time required for solublization (seconds)	Hygroscopicity (gm/100gm)
1	32	0.34	0.42	56	67
2	43	0.24	0.30	49	56
3	48	0.25	0.28	42	63
4	55	0.25	0.29	38	53
5	52	0.24	0.34	36	61
6	56	0.32	0.35	30	66
7	59	0.28	0.35	48	64
8	63	0.23	0.27	45	36
9	62	0.26	0.32	38	49
10	46	0.28	0.34	42	56
11	56	0.23	0.28	39	48
12	56	0.28	0.26	35	56
13	64	0.22	0.23	32	27
14	65	0.20	0.22	30	25

Figure 1 Effect of various spray drying parameters on % yield

Figure 2 Effect of various spray drying parameters on moisture content

Figure 3 Effect of various spray drying parameters on bulk density.

Figure 4 Effect of various spray drying parameters on time required for solubilization.

Figure 5 Effect of various spray drying parameters on Hygroscopicity.

Optimization:

Numerical optimization was carried out for spray drying process to obtain cadamba leaves aqueous extract powder. Table 1 and 2 indicates that independent variables show a complex relationship with the responses. The optimum drying conditions was determined by superimposing the contour plots of relevant responses to find out the optimized points. The following limits were proposed: yield of not less than 50%, bulk density of not more than 0.30gm/mL, moisture content of at a range of 0.2 –0.25 %, hygroscopicity of not more than 50 gm /100 gm, time required for solubilization not more than 40 seconds¹.

Figure 6 Superimposed contour plots showing powder properties affected by % of drying agent and Air Inlet Temperature

Superimposed contour plots shows the ranges of variables which could be considered as the optimum range as shown in Figure 6. The optimum ranges of variables obtained from the superimposed contours were 140 °C of inlet air temperature and 10 % of drying agent (aerosil) concentration. These optimum conditions can be used to produce cadamba leaves extract powder.

DISCUSSION:

The inlet air temperatures and % of drying aids affected the quality of cadamba leaves aqueous extract powder obtained by spray drying using Aerosil as a drying aid. Moisture content, bulk density of cadamba leaves extract powders decreased with increasing inlet air temperature. Yield increased with increasing drying aids concentration. The cadamba leaves extract powder can be obtained by spray drying process at 140°C inlet air temperature and 10 % aerosil as a drying aid.

ACKNOWLEDGEMENT:

The authors are grateful to the authorities of Dr. D.Y. Patil Institute of Pharmaceutical Sciences & Research, Pimpri, Pune for the facilities.

CONFLICT OF INTEREST:

The authors declare no conflict of interest.

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Received on 21.03.2019 Modified on 18.04.2019

Research J. Pharm. and Tech 2019; 12(8): 3886-3890.

DOI: 10.5958/0974-360X.2019.00668.1

Aerosil is used as spray drying agent for preparation of herbal extract obtained from different plants like Tanacetum parthenium18, Psidium guajava19, Mikania glomerata20, Glycyrrhiza glabra21, Ilex paraguariensis22, Maytenus ilicifolia23.

Aerosil is used as spray drying agent for preparation of herbal extract obtained from different plants like Tanacetum parthenium¹⁸, Psidium guajava¹⁹, Mikania glomerata²⁰, Glycyrrhiza glabra²¹, Ilex paraguariensis²², Maytenus ilicifolia²³.