Topic of lecture:Topic of lecture:

TINCTURES.TINCTURES.

Methods obtaining of Methods obtaining of tinctures.tinctures.

Tinctures

are referred to galenicals obtained by extraction of plant raw material (crude drugs) with an appropriate solvent.

The main object of manufacturing process is separation of the soluble principles from drugs by treating them with a liquid capable of dissolving them, which is called the menstruum or extragent.

TincturesTinctures

– – is a liquid alcohol or water-alcohol extract are is a liquid alcohol or water-alcohol extract are obtained from dried or fresh plant or animal obtained from dried or fresh plant or animal raw materials, while production of which heat raw materials, while production of which heat and remove of the and remove of the solution for extraction solution for extraction are are not carried out. not carried out.

At the manufacture of tinctures from 1 mass part At the manufacture of tinctures from 1 mass part of PRM you can produce 5 volume parts of of PRM you can produce 5 volume parts of finished product, from a potent drug – 10 finished product, from a potent drug – 10 parts. parts.

Advantages of tincturesAdvantages of tinctures

Ethanol is able to dissolve substances which are Ethanol is able to dissolve substances which are less soluble in water, while at the same time the less soluble in water, while at the same time the water content can dissolve the substances less water content can dissolve the substances less soluble in ethanol. soluble in ethanol.

It is possible to vary the proportion of ethanol It is possible to vary the proportion of ethanol and water to produce tinctures with different and water to produce tinctures with different qualities because of different substances. qualities because of different substances.

The solvent also acts as a preservative.The solvent also acts as a preservative.

Methods obtaining of tincturesMethods obtaining of tinctures

1. Maceration and its improved types 1. Maceration and its improved types

2. Percolation 2. Percolation

3. Dissolution of soft and dry extracts3. Dissolution of soft and dry extracts

Maceration

This method of tinctures production is officially used in the case of resins, balsams, gums, soap, etc., where the practical difficulties likely to be encountered in percolation would offset any advantages that the latter process might possess.

Stages of the macerationStages of the maceration::1. Loading of crushed PRM with the prescribed volume of 1. Loading of crushed PRM with the prescribed volume of

extragent in the tank for maceration and allowed to stand extragent in the tank for maceration and allowed to stand

at room temperatureat room temperature 15 – 20 °C, with frequent agitation . 15 – 20 °C, with frequent agitation .

If there are not special instructions, the infusion continues If there are not special instructions, the infusion continues during 7 days. during 7 days.

2. The mixture then is strained, the marc (the damp solid 2. The mixture then is strained, the marc (the damp solid

material) is pressed,material) is pressed, washing raw by a small volume of washing raw by a small volume of extragent, wring out again. extragent, wring out again.

3. Flowing3. Flowing together all infusions and communicating by together all infusions and communicating by solution for extraction to the desired volume.solution for extraction to the desired volume.

4. The combined liquids are clarified by filtration or 4. The combined liquids are clarified by filtration or

decantation after standingdecantation after standing..

Disadvantages of maceration: this method is slow, raw material is not fully exhausted.

Methods of intensify of the maceration:

1. Repeated maceration (bismaceration)

2. Maceration with forced circulation of extragent

3. Vortex extraction (turboextraction)

4. Ultrasound maceration

5. Maceration in the medium of milling (bolls mill and rotating pulsation apparatus are used)

Repeated maceration

may be more efficient than a single maceration, since an appreciable amount of active principle may be left behind in the first pressing of the marc.

The repeated maceration is more efficient in cases where active constituents are more valuable.

Double maceration is used for concentrated infusions which contain volatile oil, e.g.

Bismaceration or repeated maceration.

Dividing of the total volume of the extragent on 3 or 4 parts and successively infusing of the PRM with each parts of the menstruum.

Each time the extracts are poured out and flowed together.

Maceration with circulation of the

extragent. It is performed in the tank 1 for

maceration with a perforated bottom 3, on which there is the filter material 2.

4 – pump.

Solution for extraction (extragent) is smoothed through PRM which is on perforated bottom by the pump (4) for the several times to achieve of the equilibrium.

Vortex extraction

or turboextraction, is based on using of turbine stirrer which is rotates with speed about 8000 – 13 000 times for 1 minute.

Turbine stirrer causes very intensive mixing of raw material with the extragent and crushing of raw material.

Extraction time is shortened to 10 min.

Ultrasonic extraction.

The procedure involves the use of ultrasound with frequencies ranging from 20 kHz to 2000 kHz; this increases the permeability of cell walls and produces cavitation.

Source of ultrasound is attached to the body of the tank and immersed in the medium of the extraction.

Pressure with variable, cavitation and "wind sound“ are created due ultrasound.

Digestion is the form of maceration which consists in the

application of a gentle heat to the substance which is being treated.

It is used in those cases where a moderately elevated temperature is unobjectionable; the heat increases the solvent powers of the menstruum.

If the solvent or menstruum is volatile it is necessary to attach a reflux condenser to the vessel in which the lotion is being conducted so that the solvent may be recovered and returned.

Percolation (from Lat. Percolation (from Lat. RerRerccolatioolatio - filtering - filtering through)through) is the method obtaining of extracts is the method obtaining of extracts while simultaneous loading of the extragent while simultaneous loading of the extragent

and pouring out of the extract. and pouring out of the extract.

StagesStages of the P of the Percolation: ercolation:

1.1. Moistening of plant Moistening of plant raw material (swelling materials)raw material (swelling materials), 4-, 4-8 hours 8 hours

2.2. InfusionInfusion, , 24-48 hours24-48 hours

3. 3. ObtainObtaining the ing the extract by simultaneous loading the extract by simultaneous loading the extragent and pouring out of the extract.extragent and pouring out of the extract.

Percolator (a narrow, cone shaped vessel open at both ends) Percolator (a narrow, cone shaped vessel open at both ends) is used.is used.

Percolators

Moistening

The solid ingredients are moistened with an appropriate amount of the specified menstruum and allowed to stand for approximately 4 h in a wellclosed container, after which the mass is packed and the top of the percolator is closed.

Infusion

Additional menstruum is added to form a shallow layer above the mass, and the mixture is allowed to macerate in the closed percolator for 24-48 h.

Raw material is poured over with the extragent to creation a "mirror” - thickness layer of solution above the raw material which should be 30 - 40 mm

Obtaining tinctures

The inlet and outlet of the percolator are opened and the liquid contained therein is allowed to drip slowly and additional menstruum is added as required, until the percolate measures about three-quarters of the required volume of the finished product.

The mixed liquid is clarified by filtration or by standing followed by decanting.

Actually percolationActually percolation ((obtainobtaining infusing)ing infusing)

continuous continuous passage of extragent through the layer of raw passage of extragent through the layer of raw material and the collection of the extract. material and the collection of the extract.

At the same time pouring out of the extract and loading of At the same time pouring out of the extract and loading of extragent from top on PRM are conducted at speeds 1 / extragent from top on PRM are conducted at speeds 1 / 24 or 1 / 48 (for large enterprises) of working volume of 24 or 1 / 48 (for large enterprises) of working volume of percolator for 1 hour. percolator for 1 hour.

Extract is forced from PRM by flow of fresh extragent, and Extract is forced from PRM by flow of fresh extragent, and difference of concentration of BAS is create in PRM and difference of concentration of BAS is create in PRM and in extragent. in extragent.

Percolations rate should be such that diffusion of extractive Percolations rate should be such that diffusion of extractive

BAS in the extract has enough time.BAS in the extract has enough time.

The success of the process of percolation largely depends on the regulation of the flow of the percolate; if this is too rapid, incomplete exhaustion will result, but if too slow, valuable time is wasted and considerable loss of menstruum occurs from evaporation.

For fluid extracts using 1000 Gm. of powder, and rate of flow should not exceed 10 drops a minute; for official quantities of tinctures and preparations of about the same strength, 20 drops a minute

Clarifing of extracts

Extracts are a muddy liquid, containing a significant amount of suspended particles.

Extracts are clear by standing at above 10 °C to obtain of a transparent liquid.

After standing more than 2 days they era filtered by decantation (without shaking sediment).

Filterpress, Drook filters, Nootch filters, centrifuges are used for filtration.

Dissolution of Dissolution of softsoft or dry extracts or dry extracts

1. 1. Calculated amount of dry or soft extract is Calculated amount of dry or soft extract is dissolved in alcohol with required concentration dissolved in alcohol with required concentration in a reactor with stirrer. in a reactor with stirrer.

2. The obtained tinctures are filtered. 2. The obtained tinctures are filtered.

This method is characterized by a significant This method is characterized by a significant reduction in the time of tinctures obtaining. It is reduction in the time of tinctures obtaining. It is very simple, are used small number of very simple, are used small number of equipment.equipment.

The tincture is prepared by dissolving or The tincture is prepared by dissolving or diluting an extract, using alcohol of diluting an extract, using alcohol of appropriate concentration. appropriate concentration.

The content of alcohol and constituents or, The content of alcohol and constituents or, where applicable, the content of alcohol and of where applicable, the content of alcohol and of dry residue correspond to that of tinctures dry residue correspond to that of tinctures obtained by maceration or percolation.obtained by maceration or percolation.

Quality control:Quality control:

1. Appearance. Color, odor, opacity of the tincture are to be tested.

2. Relative density Where applicable, the tincture complies with the limits prescribed in the monograph.

3. Ethanol content The ethanol content complies with that prescribed. It's determined by distillation method.

4. Methanol and 2-propanol Not more than 0.05 per cent.

5. Dry residue Where applicable, the tincture complies with the limits prescribed in the monograph.

6. Identity. This test is carried out by chemical reactions (assays) and by chromatography

7. Quantitative determination of BAS.

8. Heavy metals. Not more than 0.001%.

9. Microbiological purity.