am0207_extraction method for solid food_widiastuti setyaningsih

8/8/2019 AM0207_Extraction Method for Solid Food_Widiastuti Setyaningsih

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Widiastuti SetyaningsihEuropean Master in Quality Analytical in Laboratory

Gdansk University of Technology

E-mail [email protected]

Mobile +48889664465 or +6287878121767

AM0207-EXTRACTION METHOD FOR SOLID FOOD

Date : June 03, 2010Supervision : Professor Enrique Durn Guerrero

Optimization and Comparison of Different Extraction Techniquesfor Sanguinarine and Chelerythrine in Fruits of

Macleaya Cordata (Willd) R. Br.

Researcher teamFei Zhanga, Bo Chena, Song Xiaoa, and Shou-zhuo Yaoa

PublisherSeparation and Purification Technology 42 (2005) 283290

The Purpose of Study To examine different extraction (MAE, UAE) methods for M. cordata (Willd) R. Br. To compare the relative merits of different extraction methods for M. cordata (Willd) R. Br.

Sample KnowledgeMacleaya cordata (Willd) R. Br., a poisonous plant with has the function of detumescence, detoxification andpesticide by the bio-active alkaloids content. The main components of the alkaloids are sanguinarine,chelerythrine, protopine and allocryptopine. Selection of appropriate extraction method is important to obtainthese desired compound.

Analyte KnowledgeSanguinarine (SAN) and chelerythrine (CHE) are known as major effective componentsin the quaternary benzo[c]phenanthridine isoquinoline alkaloids (QBA) fraction ofMacleaya cordata (Willd) R. Br. but possess different biological activities.

Sanguinarine, 13-Methyl-[1,3]benzodioxolo[5,6-c]-1,3-dioxolo[4,5-i] phenanthri-dinium,a quaternary ammonium salt from the group of benzylisoquinoline alkaloids.

Chelerythrine, 1,2-dimethoxy-12-methyl[1,3]benzodioxolo[5,6-c] phenanthridin-12-ium,a poisonous, crystalline alkaloid, slightly soluble in alcohol; it is derived from the seedsof the herb celandine (Chelidonium majus) and has narcotic properties.

Experimental Scheme to Compare the Extraction Efficiency

Macleaya cordata (Willd) R. Br. Filtration

0.45mDefine the Pulverization EffectMEA, UEA : Not Significantly Different

Extraction Optimization Determination Analysis 4 Times Replications High Performance Liquid Chromatography

Flow Rate 1 mL min-1, Temp. 30oC, UV detection 270 nm

Dilution Injection Volume 5lInto 100 mL with H2O
mailto:[email protected]:[email protected]


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Comparison of the Extraction :Microwave-Assisted Extraction (MAE) and Ultrasound-Assisted Extraction (UAE)

No. ParametersComparison

MAE UAE

1 Description The principle of heating usingmicrowave is based upon its direct

impact with polar materials or solventsand is governed by two phenomenons:ionic conduction and dipole rotation,which in most cases occurssimultaneously

The process of heating solvents incontact with a sample with microwaveenergy to partition compounds ofanalytical interest from the samplematrix into the solvent.

A typical maceration process with theapplication of ultrasounds and primarily

associated with cell disruption ordisintegration

When sonicating liquids at high inten-sities, the sound waves that propagateinto the liquid media result in alternatingcompression and rarefaction cycles,with rates depending on the frequency.

Ultrasonic energy breaks intermolecularbonds and releases analyte into thesolvent

Comment

The ultrasonic field enables generation, locally, of micro-cavitations in the liquid surrounding the plant material.The use of microwave energy for the extraction of active substances from plant materials results in moreeffective heating, faster energy transfer, reduced thermal gradients, selective heating, reduced equipment size,faster response to process heatingcontrol, faster start-up and increased production.

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2 Instrumentationand Radiation

Commercial WP700 microwave oven

Maximal power : 700 W

Microwave: radiation with lower energythan visible and IR radiation

Performed with an ultrasonic bath

Maximal Power : 250 W

Ultrasounds: radiation with lower energythan visible, IR and microwave radiation

Comment

Like classic extraction, intensification methods of extraction needs special equipment to be functional, whichmeans higher investments, and electricity to produce the ultrasonic and microwave waves. But, the ultrasonicsave the energy due to the radiation of ultrasonic is lower than microwave.

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3 Advantages The driving force for extraction is not

limited to the diffusion process, but ituses 'in core' heating inside the sampleto release compounds from the matrix.

Since microwave energy is selectivelydeposited in the target sample and notin the surrounding solvent, the solidstays relatively cool, leading to energyefficiency and reduced heat.

Cold extraction - good for thermallylabile compounds

Faster than MEA in extraction time dueto higher surface contact area

The ultrasonic procedure is safer thanMEA as it requires no high pressure ortemperature.

The whole procedure is simpler thanMEA and less prone to contamination

Comment

In order to increase process productivity, yield and quality of products, microwave or ultrasonic fields wereassociated with extraction of plants active compounds. From these, ultrasound assisted and microwaveextractions emerged as two promising techniques from an economical point of view, being inexpensive, simpleand efficient.

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MAE UAE

4 Disadvantages Overexposure under microwave maybecauses the loss of sample.

If higher extraction rate is needed, moreamount of solvent should be added.

Organic solvent at relative high tempe-

rature and pressure may corrode theequipments esp. the extraction vessel.

Physically violent process, may causebreakdown of macromolecules

O2 from air is going to be dissolved inthe solvent may promote the oxidation

The procedure is less robust than MEA

since ageing of the ultrasound probesurface can alter extraction efficiency

Comment

The need for development of existing methods of extraction for high effectiveness must be seriously felt. Moreresearch is needed to improve the understanding of extraction mechanism, remove technical barriers, improvethe design and scale up of the novel extraction systems for their better applications.

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5 ExtractionMethod

Dried Fruit1 gram

Dissolution100 mL of 0.1 mol L -1 HCl(aq)

Extraction Optimization

Microwave Oven, 5 minutesPower : 280; 420; 560; 700 (W)

Microwave Oven, 280 WExtraction time 1; 2; 5; and 10 minutes

Microwave Oven, 5 minutes, 280 WExtractant Volume 50; 75; 100; 125; and 150 mL

Filtration

0.45 mm

Extracted CompoundSanguinarine and Chelerythrine

Dried Fruit1 gram

Dissolution100 mL of 0.1 mol L -1 HCl(aq)

Immersion and Extraction OptimizationMaceration, 100 mL, 100oC, 30 minOptimization of Extraction Solvent

Formic Acid; Acetic Acid; Phosphoric Acid;Sulfuric Acid; Hydrochloric Acid

Maceration, 100oCExtraction Time 10; 20; 30; 40; 50 and 60 minutes

Ultrasonic Bath, 250 WExtractant Volume 50; 75; 100; 125; and 150 mL

Filtration0.45 mm

Extracted CompoundSanguinarine and Chelerythrine

Comment

For microwave extraction, the power of irradiation must be chosen correctly among 280; 420; 560; and 700Watt to avoid excessive temperature, which could lead to solute degradation and overpressure inside thevessel. It was defined 250 W as irradiation power in ultrasonic extraction.

A proper study on optimization of extraction time is vital because extraction time may vary with different plantpart used. Generally, by increasing the extraction time, the quantity of analytes extracted is increased, althoughthere is the risk that degradation may occur. In this study, microwave extraction investigated during 1, 2, 5 and

10 minutes whereas ultrasonic was conducted at 10, 20, 30, 40, 50 and 60 minutes as maceration extractiontime optimization.

A higher ratio of solvent volume to solid matrix may effective in ultrasonic extraction methods. However, in MAEa higher ratio may yield lower recoveries, which may be due to inadequate stirring of the solvent by microwaves

A correct choice of solvent is fundamental for obtaining an optimal extraction process. Preferably the solventshould have a high selectivity towards the analyte of interest excluding unwanted matrix components.

Since the base operating time in microwave for other optimizations is only 5 minutes whereas ultrasonic has 30minutes, the extraction optimization process of microwave is faster than the ultrasonic.

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MAE UAE

6 ExtractionOptimization

Optimum Parameters Setting, i.e.

Irradiation power : 280 W

Extraction time : 5 minutes

Extractant volume : 100 mL

Extractant Solution : 0.01 mol L-1 HCl

Optimum Parameters Setting, i.e.

Irradiation power : 250 W

Extraction Time : 30 minutes

Extractant volume : 100 mL

Extractant Solution : 0.1 mol L-1 HCl

Comment

Microwave power and irradiation time are two such factors, which influences each other to a great extent. Acombination of low or moderate power with longer exposure may be a wise approach. In this study, it wasdefined the irradiation power for microwave extraction in the lowest level (280 W) which is nearby with theirradiation power for ultrasonic extraction.

In microwave extraction, 5 min was selected as the optimum extraction time, since this was sufficient to extractthe target alkaloid present in samples ofMacleaya cordata (Willd) R. Br. Whereas ultrasonic extraction needs30 minutes to achieve optimum recovery of the analytes. Therefore, in extraction time, Microwave extractionwas faster than ultrasonic extraction.

Volume of the extracting solvent is also a critical factor. The overall knowledge is that the solvent volume mustbe sufficient to ensure that the Macleaya cordata (Willd) R. Br. matrix is always entirely immersed in the solventthroughout the entire irradiation time. The volume for both extraction was the same as much as 100 mL. Thereis no significant different in increasing of extraction efficiency from 100 mL to 150 mL.

Solvent choice was dictated by the solubility of the target analyte, by the interaction between solvent and

Macleaya cordata (Willd) R. Br. Matrix. The extraction efficiency of formic and acetic acid to alkaloids is low dueto the limitation of their acidity. When pH was maintained around 1, the extraction efficiency of H 2SO4(aq) andH3PO4(aq) to alkaloids was lower than HCl (aq). Therefore, HCl(aq) was selected as extracting solvent in followingexperiments. Generally, the extracting efficiency of HCl (aq) for alkaloids increases with the increasing of the acidconcentration. But when the concentration of HCl (aq) was 0.01 mol/l, the efficiency of microwave extraction wasmuch more higher than maceration extraction. It shows that microwave extraction is more effective extractionmethod than maceration extraction.

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MAE UAE

7 Recovery

The salmon color of shadow shows the alkaloid recovery which is extracted usingMicrowave-assisted extraction and ultrasound-assisted extraction.

Fingerprint chromatograms of extractsobtained using microwave-assistedextraction techniques

Fingerprint chromatograms of extractsobtained using ultrasound-assistedextraction techniques

Comment

Microwave-assisted extraction gave significantly higher value of alkaloid recovery (mg g -1 sample) thanultrasound-assisted extraction. This sonication extraction have extraction capabilities and limitations owing totheir inherent and unique features (see disadvantages in point no.4).

Fingerprint chromatograms of extracts obtained to compare between microwave-assisted extraction andultrasound-assisted extraction. It shown if there is a difference on fingerprint characteristic from 3 to 10 minutesof retention time, special on relative abundance of peaks.

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Conclusion

The majority of extraction procedures for the determination of plant metabolites are developed in such a waythat the final extract introduced into the HPLC columns contains only the analytes with all interferencesremoved.

From the total grade that is mentioned bellow which was obtained from individual sum in each parameters,shows that microwave-assisted (4 value) is better than ultrasound-assisted extraction (1 value). Where in thisstudy, it was proofed if microwave-assisted extraction was more effective compare to ultrasound-assistedextraction. Besides, the main advantaged of microwave-assisted extraction than ultrasound-assisted extractionare shorter extraction times (typically 5 minutes) and less use of solvent concentration (0.01 mol L-1 HCl(aq)).

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am0207_extraction method for solid food_widiastuti setyaningsih

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