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PHARMACEUTICAL STANDARDIZATION
Year : 2014  |  Volume : 35  |  Issue : 1  |  Page : 63-70  

Process standardization and characterization of Rajata Sindura


1 Department of Rasa Shastra and Bhaishjya Kalpana, Mahatma Gandhi Ayurved College, Hospital and Research Centre, Wardha, Maharashtra, India
2 Department of Dravyaguna, Mahatma Gandhi Ayurved College, Hospital and Research Centre, Wardha, Maharashtra, India
3 Department of Rasa Shastra and Bhaishjya Kalpana, Government Ayurveda Medical College, Bengaluru, Karnataka, India

Date of Web Publication29-Sep-2014

Correspondence Address:
Rohit A Gokarn
Department of RS and BK, Mahatma Gandhi Ayurved College, Hospital and Research Centre, Wardha, Maharashtra - 442 001
India
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Source of Support: None, Conflict of Interest: None


DOI: 10.4103/0974-8520.141940

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   Abstract 

Background: Rajata Sindura (RS) is a mercurial preparation, known for its properties like Rasayana (rejuvinating), Balya (strengthening), Vrushya (aphrodisiac), Medhya (increasing intellect) and can cure various diseases when used with appropriate adjuvant. It is prepared with Hingulottha Parada (purified mercury), Shuddha Gandhaka (purified sulfur) and Shuddha Rajata (purified silver) in a proportion of 1:1:4. Process standardization and characterization of RS are not reported until date. Aim: Pharmaceutical standardization and characterization of Rajata Sindura. Materials and Methods: Purified mercury and silver were triturated to form amalgam, followed by the addition of purified sulfur to prepare Kajjali and lavigated with Vatankura (leaf buds of Ficus benghalensis Linn.) swarasa (juice). This Kajjali was processed by Kupipakwa method. Results and Conclusion: RS was prepared in 33 h with 20.25% yield. Scanning electron microscope coupled with energy dispersive spectroscopy analysis has shown Mercury 86.21%, sulfur 13.27% as major elements; iron, calcium, potassium, magnesium and silver were other detected minor elements. X-ray diffraction report revealed the chemical nature of RS as HgS compound, having cubic crystal structure.

Keywords: Kupipakwa Rasayana , Rajata Sindura, X-ray diffraction


How to cite this article:
Gokarn RA, Gokarn SR, Hiremath SG. Process standardization and characterization of Rajata Sindura. AYU 2014;35:63-70

How to cite this URL:
Gokarn RA, Gokarn SR, Hiremath SG. Process standardization and characterization of Rajata Sindura. AYU [serial online] 2014 [cited 2020 Sep 22];35:63-70. Available from: http://www.ayujournal.org/text.asp?2014/35/1/63/141940


   Introduction Top


Rasa Shastra, an advanced pharmaceutical science describes the conversion of metals and minerals into therapeutically safe and potent forms. Rashoushdhies are herbo-mineral compound formulations, known for their quick curative attributes with small doses. [1] Kupipakwa Rasayana is one among the important formulations described under the Parada Murchana (inducing disease curing property in a drug) and is considered best in terms of its wide spectrum in therapeutics. [2] Kupipakwa Rasayana, is a unique pharmaceutical preparation where in the drug is prepared in a glass bottle (Kupi) and the processing is done in the furnace with the gradual rise of temperature. [3] Pharmaceutical preparation by Kupipakwa method enhances the property of the drug, to form a stable, safe, efficacious compound, which is evident by various studies on Rasasindura.[4],[5] Metals are also used as an ingredient in various Kupipakwa Rasayanas such as Makaradhwaja, Rajata Sindura (RS), Tamra Sindura, etc., Rajata (silver) a widely used metal in therapeutics in different forms such as Bhasma, Sindura, etc., RS contains silver, mercury and sulfur, having therapeutic potential ranging in diseases such as Madhumeha (diabetes), Jwara (fever), Hridroga (heart diseases) and also possesses Rasayana (rejuvenation) and Vajeekarana (aphrodisiac) properties. [6] Until date, no reported studies are available pertaining to standardization and characterization of RS. Hence an attempt has been made to develop pharmaceutical standardization of RS and to explore the structure and composition through sophisticated instrumental facilities like X-ray Diffraction (XRD), Scanning Electron Microscope coupled with Energy Dispersive Spectroscopy (SEM-EDX) and particle size analyzer.


   Materials and Methods Top


Raw materials

Rajata Sindura (RS) (99.97% pure) was collected from Asmita silver refinery, Bangalore. Hingula (cinnabar) and Gandhaka (sulfur) were procured from Amrita Kesari, Bangalore, and confirmed for their authenticity based on the classical parameters. [7] Vatankura (leaf buds of Ficus benghalensis Linn.) were collected form botanical garden of the Institute and Nimbu (Citrus limon Linn.) was collected from local market. Equipments like Kupi (glass bottle) coated with seven layers of mud smeared cloth with capacity of 750 ml; Bhatti (traditional furnace) measuring diameter-5 cm: Height-85 cm, upper hole- 30 × 30 cm 2 for wood: Lower hole-20 × 30 cm 2 for collecting ash, Valuka Yantra (iron vessel filled with sand for placing the Kupi) measuring diameter inner-20 cm: Brim-30 cm: Height-30 cm: Depth-27 cm: Thickness-03 cm, Valuka (sand) and wood were prepared as per the requirement.

Methods

Preparation of RS involves the following steps:

  1. Purvakarma includes purification of raw materials, preparation of Kajjali and Bhavana
  2. Pradhana Karma involves processing of drugs in furnace
  3. Paschat Karma, breaking of Kupi and collection of product.


Purvakarma

Mercury was extracted from cinnabar by Nadayantra method. [8] Initially, cinnabar was levigated with Nimbu Swarasa (juice of C. limon) and fine powder of triturated cinnabar was spread uniformly over a cotton cloth (equal to the weight of cinnabar), tied with thread and ignited. While igniting an earthen pot was placed inverted to facilitate the collection of mercury. Thus obtained mercury was collected carefully and filtered through four folded cloth [Table 1], [Figure 1]. Sulfur was purified by Dhalana method. [9] Impure sulfur was taken in a stainless steel container along with Ghrita (1/4 part) and melted over mild flame. A muslin cloth smeared with Ghrita was tied to the mouth of the container containing milk. As soon as sulfur melted, the mixture was poured through the cloth into the container containing milk. Thus obtained sulfur was washed with hot water and dried. The above process was repeated for two more times [Table 2], [Figure 2]. Samanya Shodhana of Rajata[10] was carried out by quenching in different liquids like Tila Taila (sesum oil), Takra (butter milk), Gomutra (cow's urine), Aranala (sour gruel prepared out of rice), and Kulattha Kwatha (decoction of Vigna unquiculata Linn.) as per the classical reference. Vishesha Shodhana[11] was done by Nirvapa (heating and dipping) in Nimbu Swarasa for 7 times [Table 3], [Figure 3].
Figure 1: Purified mercury

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Figure 2: Purified sulfur

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Figure 3: Purified silver

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Table 1: Extraction of mercury from cinnabar

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Table 2: Observations during purification of sulfur

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Table 3: Observations made during Samanya and Vishesha Shodhana of silver

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Preparation of Kajjali

Purified silver foils were placed in mortar containing purified mercury. Immediately trituration was carried out in mortar by using pressure till silver amalgamated completely [Figure 4]. This was added with fine powder of purified sulfur and trituration was continued until the formation of Kajjali (fine, smooth, lusterless powder). This was added with Vatankura Swarasa [Figure 5] and left over night for soaking in mortar [Figure 6]. [12] The next day trituration was done for 4 h, allowed to dry, collected and stored in a glass container [Table 4].
Figure 4: Process of amalgamation

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Figure 5: Juice of Ficus benghalensis Linn

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Figure 6: Impregnation with juice

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Table 4: Ingredients for preparation of Rajata sindura kajjali

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Pradhana Karma

Kajjali
was filled in the Kupi and kept in the Valuka Yantra [Figure 7], which was placed in the Bhatti [Figure 8]. Pyrometer was placed at the bottom of Kupi in Valuka Yantra. Fire was set; temperature reading was carried out at regular intervals of 30 min. Kramagni (gradual rise of temperature) was maintained [Graph 1 [Additional file 1]]. Corking was done after complete cessation of flame [Figure 9] and observing the Siddhi Lakshanas, like complete cessation of sulfur fumes, Suryodaya Lakshana (red appearance of the bottom) [Figure 10] and positive copper coin test, etc., [Table 5].
Figure 7: Kupi placed in Valuka Yantra

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Figure 8: Classical furnace

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Figure 9: Blue flame

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Figure 10: Red hot appearance of bottom

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Table 5: Observations during the preparation of RS

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Paschat Karma

Kupi
was left for self-cooling, layers were scraped and the bottle was broken carefully [Figure 11]. Product deposited at the neck of the Kupi was carefully collected [Figure 12] and weighed. RS was prepared in three batches to develop Standard Manufacturing Process (SMP).
Figure 11: Breaking Kupi

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Figure 12: Rajata Sindura

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Analytical study

Two samples i.e. Rajata Sindura Kajjali (RSK) and RS were analyzed for physicochemical parameters like pH value, [13] ash value, [14] acid insoluble ash, [15] water soluble ash, [16] loss on drying, [17] tests for the presence of total mercury, [18] and total sulfur containt. [19] Instrumental analysis like XRD by Philips X PERT PRO diffractometer Cu-Kα radiation (ϑ =1.5405 A°), (SEM, model JSM-6380 LA from JEOL, Japan), and particle size determination by laser scattering particle size analyzer (LA-910) using triple distilled water as a medium were carried out for characterization of RSK and RS.


   Observations and Results Top


Different phases of the desired characteristics during the process were observed viz. sulfur fuming, melting and boiling of Kajjali, blue flame, and confirmative test (flame disappearance, Shita Shalaka test, red hot appearance of bottom, copper coin test) were observed and recorded. RS collected from the neck of Kupi from all the three batches was weighed [Table 6]. Results of various organoleptic, physico-chemical parameters, XRD [Graph 2 [Additional file 2]] and [Graph 3 [Additional file 3]], SEM-EDX [Graph 4 [Additional file 4]] and [Graph 5 [Additional file 5]] and particle size were analyzed [Table 7],[Table 8],[Table 9] and [Table 10].
Table 6: Weight of Rajata Sindura

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Table 7: Results of physico‑chemical tests

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Table 8: Results of XRD

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Table 9: SEM‑EDX results of RSK and RS

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Table 10: Results of particle size determination of RSK and RS

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   Discussion Top


Extraction of mercury from cinnabar yielded 71.2%, even though cinnabar contains 86.13% of mercury, the classical method did not yield the amount of mercury up to expected quantity. The reason of loss may be due to mercurial vapors escaping out during the procedure and some amount of mercury entering the minute pores of earthen pot used for collection. However, previous work carried out on the same concluded 73% of yield from the same method. [20] During purification of sulfur, 3.8% of loss was observed. It is evident from the observation that bright yellow color and sulfurous odor was reduced after each Dhalana. During Rajata Shodhana, minimal weight loss was observed. Although silver gets tarnished by the contact of various liquid media, less corrosion was seen on silver, which is evident by the intact silver foils after process. It took 30 h to make amalgam and 120 h to make Kajjali. In Kupipakwa Rasayana, the heating pattern plays an important role to obtain a quality product. As per classical texts, Krama Vruddha Agni[21] is adopted during the process. The heating duration was divided into three equal parts i.e., 11 h each. This heating pattern was divided in to 3 stages Mridu (120-250°C), Madhayma (250-450°C) and Tivragni (450-650°) [Graph 1]. The first stage of heating represents the melting of RSK, whereas in second and third stage, boiling of RSK and sublimation of the product towards the neck of the Kupi was evident. Various tests like copper coin test, Sheeta Shalaka test were conducted to confirm the absence of free sulfur. Testing of the product collected at the neck was also done to ensure proper formation of compound. Self-cooling of Kupi was ascertained before procuring product as it has a major role to play in re-crystallization.

Specific procedure adopted in Kupi Paka and temperature pattern followed facilitates the chemical reaction. Change in chemical nature and crystalline structure was evident from XRD reports in RS (vermillion) as compared with RSK (imitrite).

According to previous research works, Rasasindura prepared in Kupi possesses HgS as cinnabar having hexagonal crystal structure [22] whereas RS has shown HgS as cubic crystal system with primitive lattice. Both Rasasindura and RS possess same chemical formula-HgS, but differ in the crystal lattice. Change in the crystal structure can occur due to embedded metal ion in crystal system. [23] Here, silver ions present in the crystal lattice may be responsible to change the crystal structure.

RS revealed HgS compound in XRD study, by comparing with XRF results one can validate the analysis as the percentage of Hg (86.21%) and S (13.27%) are stoichiometrically accurate to that of theoretical calculation in HgS compound. Inclusion of minor and trace elements such as Mg (0.11), P (0.12), K (0.02), Ca (0.07) and Fe (0.1) may be due to the impregnation of Vatankura Swarasa. [24]

The RS particle size was 9.59 μm, which is slightly larger than Kajjali. RS is a condensed and re-crystallized product under high temperature and pressure, so segregation of particle may be responsible for the increase in particle size; however, it also depends on the trituration undertaken while sampling.


   Conclusion Top


Rajata Sindura (RS) can be prepared in 33 h by following intermittent gradual rise of temperature, i.e. 11 h each of Mridu (120-250°C), Madhyama (250-450°C) and Tivragni (450-650°C) with 20.25% yield. RS is a mercurial compound possesses HgS with cubic crystal structure with Hg 86.21%, S 13.27% as major elements and Fe, Ca, K, Mg and Ag as minor elements.

 
   References Top

1.Somadev, Rasendra Chudamani, 1/33, 3 rd ed, Chaukhamba Orientalia, Varanasi, 2004; 9.  Back to cited text no. 1
    
2.Madhava, Ayurveda Prakasha, 1/137, Chaukhamba Bharati Academy, Varanasi, 2007; 80-1.  Back to cited text no. 2
    
3.Dwivedi V. Bharateeya Rasashastra. 2 nd ed., 8. Nagpur: Shri Sharma Ayurved Mandir; 1987. p. 224.  Back to cited text no. 3
    
4.Singh SK, Chaudhary AK, Rai DK, Rai SB. Preparation and characterization of a mercury based Indian traditional drug Rasasindo or. Indian J Tradit Knowl 2009;8:346-57.  Back to cited text no. 4
    
5.Dwivedi V, Anandan EM, Mony RS, Muraleedharan TS, Valiathan MS, Mutsuddi M, et al. In vivo effects of traditional Ayurvedic formulations in Drosophila melanogaster model relate with therapeutic applications. PLoS One 2012;7:e37113.  Back to cited text no. 5
    
6.Sharma H. Bhaishajya Sara Sangraha. Ahmadabad: Unjha Pharmacy Ltd.; 1955. p. 304.  Back to cited text no. 6
    
7.Somadev, Rasendra Chudamani, 14/30, 3 rd ed., Chaukhamba Orientalia, Varanasi, 2004; 237.  Back to cited text no. 7
    
8.Bhatta RK. Siddha Bhaishajya Manimala, 5/4. 4 th ed. Varanasi: Krishna Das Academy; 1999. p. 355.  Back to cited text no. 8
    
9.Vagbhata, Rasaratnasamuchchaya, 3/20, 2 nd ed., Meharchanda Lachmandas, Delhi, 2010; 45.  Back to cited text no. 9
    
10.Ibidem, Rasaratnasamuchchaya, 5/13; 93.  Back to cited text no. 10
    
11.Sharma S. Rasa Tarangini, 16/6-12. 11 th ed. New Delhi: Motilal Banarsidas Press; 2004. p. 387.  Back to cited text no. 11
    
12.Govindadas, Bhaishjya Ratnavali, 4/117, 18 th ed., Chaukhamba Samskrit Samsthan, Varanasi, 2005; 61.  Back to cited text no. 12
    
13.Anonymous. The Ayurvedic Pharmacopoeia of India. 1 st ed., Vol. 2, Part 2, Appendix 3 (3.3). New Delhi: Govt. of India: Ministry of Health and Family Welfare; 2006. p. 212.  Back to cited text no. 13
    
14.Ibidem. The Ayurvedic Pharmacopoeia of India, Vol. 2, Part 2, Appendix 2 (2.2.3); p. 159.  Back to cited text no. 14
    
15.Ibidem. The Ayurvedic Pharmacopoeia of India, Vol. 2, Part 2, Appendix 2 (2.2.4); p. 159.  Back to cited text no. 15
    
16.Ibidem. The Ayurvedic Pharmacopoeia of India, Vol. 2, Part 2, Appendix 2 (2.2.5); p. 159.  Back to cited text no. 16
    
17.Ibidem. The Ayurvedic Pharmacopoeia of India, Vol. 2, Part 2, Appendix 2 (2.2.10); p. 161.  Back to cited text no. 17
    
18.Ibidem. The Ayurvedic Pharmacopoeia of India, Vol. 2, Part 2, Appendix 5 (5.2.7); p. 269.  Back to cited text no. 18
    
19.Ibidem. The Ayurvedic Pharmacopoeia of India, Vol. 2, Part 2, Appendix 5 (5.2.11); p. 270.  Back to cited text no. 19
    
20.Mehta NJ, Patgiri BJ, Prajapati PK. Standard operating procedure of Hingulottha Parada. Int J Ayurvedic Med 2010;1:27-36.  Back to cited text no. 20
    
21.Dasondi M, Singh K, Patgiri BJ, Ravishankar B, De S. A comparative pharmaco-chemical study of Samaguna and Shadaguna Balijarita Rasa Sindhoora w.s.r.to its toxicity. Jamnagar: IPGT and RA, Gujarat Ayurved University; 2002.  Back to cited text no. 21
    
22.Yadav P, Vyas M, Dhundi S, Khedekar S, Patgiri BJ, Prajapati PK. Standard manufacturing procedure and characterisation of rasasindoora. Int J Ayurvedic Med 2011;2:72.  Back to cited text no. 22
    
23.How do impurities affect the structure and properties of a solid. Available from: http://www.science. uwaterloo.ca/~cchieh/cact/applychem/defect.html. [Last accessed on 2011 July 23].  Back to cited text no. 23
    
24.Khan KY, Khan A, Niamat R, Shah GM, Fazal H, Seema N, et al. Elemental content of some anti-diabetic ethnomedicinal species of genus Ficus Linn. using atomic absorption spectrophotometry technique. J Med Plants Res 2012;6:2136-40.  Back to cited text no. 24
    


    Figures

  [Figure 1], [Figure 2], [Figure 3], [Figure 4], [Figure 5], [Figure 6], [Figure 7], [Figure 8], [Figure 9], [Figure 10], [Figure 11], [Figure 12]
 
 
    Tables

  [Table 1], [Table 2], [Table 3], [Table 4], [Table 5], [Table 6], [Table 7], [Table 8], [Table 9], [Table 10]



 

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