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Table of Contents
ORIGINAL ARTICLE
Year : 2020  |  Volume : 8  |  Issue : 3  |  Page : 210-216

Shelf-life evaluation of Indukanta Ghritam: A preliminary study


Department of Rasa Shastra and Bhaishajya Kalpana, All India Institute of Ayurveda (AIIA), New Delhi, India

Date of Submission04-Aug-2020
Date of Decision22-Sep-2020
Date of Acceptance01-Oct-2020
Date of Web Publication11-Nov-2020

Correspondence Address:
Dr. Punam Aggarwal
Department of Rasa Shastra and Bhaishajya Kalpana, All India Institute of Ayurveda (AIIA), Mathura Rd, Gautampuri Awas, Sarita Vihar, New Delhi.
India
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Source of Support: None, Conflict of Interest: None


DOI: 10.4103/JISM.JISM_77_20

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  Abstract 

Background: The concept of Saviryata Avadhi (shelf life) of different Ayurveda dosage forms is well described in Sharngadhara saṃhita. Shelf life is an important component and is mandatory to be displayed on the label of all medicinal products. This is also applicable to Ayurveda; thus, it becomes essential to establish shelf life of formulations that are being marketed and used in therapeutics. An attempt has been made in this study to evaluate shelf life of Indukanta Ghritam (IKG) which is not reported till date though in general it has been quoted by Gazette of India, that is, 2 years. Aim: To evaluate the shelf life of IKG through the accelerated stability study. Materials and Methods: Five batches were prepared according to Ayurveda Pharmacopoeia of India and the observations and results were systematically recorded. Physicochemical parameters were measured at the temperature of 40°C ± 2°C and the relative humidity was 75% ± 5%. The analysis was carried out at the intervals of 0, 1, 3, and 6 months, and the average 10% degradation time was calculated and extrapolated to find the shelf life as per ICH guidelines and high-performance thin-layer chromatography (HPTLC) analysis of sample was also carried out. Results: The average percentage loss in final product was 7.71% in IKG. The shelf life of IKG is found to be 19 months. Conclusion: The classics have mentioned the shelf life as 16 months, whereas the Gazette of India states the shelf life as 2 years for Ghrita. The shelf life of IKG is equal to the classic. This might be because of the precautions observed during the manufacturing and storing phases of the drug.

Keywords: Indukanta Ghritam, Saviryata Avadhi, shelf life, stability study, Yogratnakara


How to cite this article:
Aggarwal P, Ruknuddin G, Prajapati PK. Shelf-life evaluation of Indukanta Ghritam: A preliminary study. J Indian Sys Medicine 2020;8:210-6

How to cite this URL:
Aggarwal P, Ruknuddin G, Prajapati PK. Shelf-life evaluation of Indukanta Ghritam: A preliminary study. J Indian Sys Medicine [serial online] 2020 [cited 2020 Dec 1];8:210-6. Available from: https://www.joinsysmed.com/text.asp?2020/8/3/210/300498




  Introduction Top


Shelf life (Saviryata Avadhi) means how long the drug remains potent or have action for which it has been mentioned/reported. It can be defined as length of time, after which substances start to degrade in their qualities Rasa (taste), Guna (property), Veerya (potency), Vipaka (bio transform), and become unsuitable for consumption or sale. To precise shelf life of a product guarantees full potency and safety of a drug. Most medications, continue to be effective and safe for a time after the expiration date. It is often mathematically modeled around a parameter such as the concentration of a chemical compound, a microbiological index, or moisture content.[1]

In Samhita kala, description about storage of finished product is not mentioned but specific Sangraha vidhi of raw materials which is used as it is for treatment or used for specific formulations is described.[2],[3],[4] The shelf-life period is mentioned in texts such as Vangasena,[5] Sharangadhara samhita,[6] and Yogaratnakara[7] for different Ayurveda dosage forms.

The Saviryata Avadhi of Ghrita given in Sarangadhara samhita is 16 months.[6] Shelf life defines for Ghrita according to Rule 161-B, Drugs and Cosmetics Act is 2 years.[8]

Considering changes in the pharmaceutical scenario and storage techniques; the same concepts of shelf life cannot be implemented today. Hence, a need is felt to re-establish these concepts following the current guidelines. Published reports on this aspect are very few. With this background, it has been planned to evaluate shelf life of Indukanta Ghritam (IKG).


  Materials and Methods Top


Authentication

All raw drugs used in the preparation of IKG were authenticated at the National Institute of Science Communication and Information Resources (NISCAIR), New Delhi for its authenticity. The drug was cleaned to remove physical impurities and allowed to dry completely in shade.

Preparation of Indukanta Ghritam

IKG was prepared according to API,[9] by using authentic raw material in the Department of Rasa Shastra and Bhaishajya Kalpana, All India Institute of Ayurveda (AIIA), New Delhi. It is made up of following Dravyas (materials); Kalka Dravya (paste), Drava Dravya (liquids), and Sneha Dravya (fat and oily material) mentioned in [Table 1]. The prepared Ghrita was labeled as IKG and subjected to organoleptic and physicochemical and in order to develop preliminary analytical profiles.
Table 1: Formulation composition of Indukanta Ghritam

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Sample Quantity and Packing

IKG were packed in air tight glass containers (250mL capacity) and each four containers containing 150g of IKG were packed and stored in an accelerated stability chamber [Figures 1–5].{Figure 1}

Study Period

The study was conducted from August 2019 to February 2020.

Storage Conditions in the Stability Chamber

The accelerated stability study was conducted as per the ICH guidelines.[10] The temperature maintained during the study period was 40°C ± 2°C, whereas the relative humidity was 75% ± 5%.

Frequency of Withdrawal of the Sample

The sample was withdrawn from the stability chamber at the intervals of 0, 1, 3, and 6 months and evaluated for relevant parameters.

Physiochemical Analysis

The formulation was studied at the specified intervals for changes in organoleptic parameters including odor, taste, and physicochemical parameters including moisture content,[11] specific gravity,[12] saponification value,[13] acid value,[14] peroxide value,[15] total fatty matter, viscosity by Brookfield,[16] tests for microbial contamination,[17] and comparative high-performance thin-layer chromatography (HPTLC) fingerprinting were done initially and, at the end of 6 months, by following the standard guidelines.[18],[19]

HPTLC Fingerprinting of Indukanta Ghritam

Preparation of test solutions

0.1mL of IKG was taken in a test tube and diluted with 1mL of hexane and it was mixed well. This test solution was used for HPTLC fingerprinting.

Preparation of spray reagent (5% sulfuric acid in methanol reagent)

5mL sulfuric acid is cautiously mixed with 100mL methanol.

Mobile phase

Hexane: diethyl ether (7: 3 v/v).


  Observations and Results Top


The comparative organoleptic characters and physicochemical parameters of the IKG results obtained at different stages of withdrawal (0, 1, 3, and 6 months) are shown in [Table 2]. Microbial growth was found below prescribed limits in test drug initially and after sixth month. In IKG, absence of all pathogen and presence of total plate, yeast, and mold count were within the prescribed limits depicted in [Table 3].
Table 2: Analytical profile of Indukanta Ghritam at different intervals of accelerated stability

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Table 3: Microbial contamination initially and at the end of sixth month

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Results obtained at different stages of withdrawal (0, 1, 3, and 6 months) were analyzed to calculate intercept, slope [Table 4], and 10% degradation of IKG [Table 5]. The acceptable point to extrapolate the accelerated stability data is set as 10% degradation. The mean obtained of these months was multiplied with the real-time aging factor. As India comes under climatic zone III countries, the real-time aging factor becomes 3.33 that was used to extrapolate shelf life. The number of months when 10% degradation of the formulation occurred was calculated using the following formula: 10% degradation occurs = [0 - month assay value {0-month assay value × 10/100]}-intercept/slope. Thus, the shelf life of IKG was found to be 19 months [Table 6].
Table 4: Intercept and slope of Indukanta Ghritam

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Table 5: Approximate period for 10% degradation in Indukanta Ghritam

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Table 6: Extrapolation of shelf life in Indukanta Ghritam

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HPTLC of Indukanta Ghritam


  Discussion Top


Shelf life is a crucial component of quality control, which is also an indicator of care taken during the manufacturing, packing, and storing of raw as well as finished products. According to the Drugs and Cosmetics Act 1940, it is now mandatory to display shelf life on the label of a container of all medicinal products including Ayurveda. Thus, it becomes essential to establish shelf life of all formulations being used in therapeutics.[20]

Shelf life of Rasayana churna, Vasa avaleha, Kamsaharitaki avaleha, Shirishashwagandhadi avaleha, Hridya yoga churna, Shirisha avaleha, and Laghu sutashekhara rasa have been reported but shelf life of IKG is not reported till date.[21]

Considering the ICH guidelines, shelf life was evaluated through accelerated stability protocol.[10] Acid value indicates the presence of free fatty acid in the sample. The free fatty acid is due to hydrolysis of glycerides by the presence of moisture. The higher free fatty acid value indicates rancidity of the sample. In this study, the acid value is found to be 1.55mg/g that is nearer to the values set by API.[9] The value shows the sample is not rancid.

Peroxide value also indicates the rancidity of the preparation. It is the parameter specifying the content of oxygen as peroxide especially hydroperoxide in a substance. It is the measure of oxidation. Generally, peroxide value for a nonrancid fat/oil is less than 11 meq/kg.[9] In this study the peroxide value was found 6.43 meq which is within limits, indicating the Ghrita is not rancid.

Saponification value indicates the amount of hydrolysis of fat or oil. The Saponification value of Ghrita should not be more than 229–231g/mg.[9] In this study, the obtained saponification value is 209.190g/mg, which is less than the desired level of range.

HPTLC of IKG was done at two intervals, that is, initially and at the end of six months. The mobile phase used in this experiment was hexane: Diethyl ether (7: 3 v/v). Rf values were visualized @ 254nm which are three on each track, six on each track @ 366nm, and four on each track @ 540nm at both the intervals. There were no significant differences in between the intervals at each visualization, indicating that no much physical or chemical changes took place in the product on storage in HDPE containers for six months in accelerated atmospheric conditions [Table 7] [Figure 6],[Figure 7],[Figure 8],[Figure 9],[Figure 10],[Figure 11].
Table 7: Rf values of Indukanta Ghritam at different wavelengths

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Figure 6: 3D overlay chromatogram @254 nm

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Figure 7: HPTLC plate @254 nm

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Figure 8: 3D overlay chromatogram @366 nm

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Figure 9: HPTLC plate @366 nm

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Figure 10: 3D overlay chromatogram @540 nm

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Figure 11: HPTLC plate @540 nm

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The formulation was analyzed for microbial contamination including total plate count, total yeast and mold count, and four pathogens (Escherichia coli, Pseudomonas aeruginosa, Staphylococcus aureus, Salmonella). Absence of pathogen and presence of total plate, yeast, and mold count were within the prescribed limits. [Table 3] indicates that IKG is free from microbial contamination. The total plate, yeast, and mold count were unchanged after storing for six months, and were within the prescribed limits [Table 3]. This reflects the care taken during the pharmaceutical process, selection of containers, and storing period. It also helps in reduction or degradation of formulation which is ultimately increasing shelf life.

Based upon intercept and slope [Table 4] and [Graph 1],[Graph 2],[Graph 3],[Graph 4],[Graph 5] and further approximate period required for 10% degradation [Table 5] were calculated. The 10% degradation was extrapolated and it has been found that the shelf life of IKG is 19 months [Table 6]. The classics have mentioned the shelf life as 16 months,[6] whereas the Gazette of India states the shelf life as 2 years for Ghrita.[8] The shelf life of IKG is equal to the classical description.
Graph 1: Viscosity by Brookfield

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Graph 2: Acid value

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Graph 3: Peroxide value

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Graph 4: Saponification value

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Graph 5: Total fatty matter

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Basic factors responsible for product degradation are temperature, humidity, microbial growth. When these factors are favorable, certain chemical reactions in between different functional groups present in the herbal material is expected. The chemical reactions may be oxidation or reduction or hydrolysis or formation of new complexes or volatilization or sublimation or phase conversion or transformation into different compounds. Moisture content plays an important role in deterioration of any substance because moisture can activate various enzymes, which leads to decompose of a product.[21] To avoid such chemical changes, precautions need to be taken at different levels of drug manufacturing.


  Conclusion Top


The classics have mentioned the shelf life as 16 months, whereas the Gazette of India states the shelf life as 2 years for Ghrita. The shelf life of IKG in this study is found to be almost equal to the classical description inferring that the standard precautions were observed during the manufacturing process and storing phases of the formulation.

Acknowledgement

The authors would like to acknowledge the support extended by the Director, All India Institute of Ayurveda (AIIA), New Delhi, and technical support extended by Vasu Pharmaceuticals, Baroda, in conducting the shelf-life analysis of the product.

Financial support and sponsorship

Nil.

Conflicts of interest

There are no conflicts of interest.



 
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    Figures

  [Figures 1–5], [Figure 6], [Figure 7], [Figure 8], [Figure 9], [Figure 10], [Figure 11], [Figure 12], [Figure 13], [Figure 14], [Figure 15], [Figure 16]
 
 
    Tables

  [Table 1], [Table 2], [Table 3], [Table 4], [Table 5], [Table 6], [Table 7]



 

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