Hielscher Ultrasound Technology

Ultrasonic Extraction of Piperine from Pepper

  • Piperine is a bioactive substance that is found in peppercorns and valued for its pharmacological properties.
  • Ultrasonic is an efficient, simple, and rapid extraction technique to isolate high-quality piperine.
  • Ultrasonic extraction is a reliable and proven method, already widely used in the pharma and food industry.

Piperine Extraction by High-Performance Ultrasound

Piperine ia a valued bioactive compound known for its potential to increase absorption of curcumin, selenium, vitamin B12, beta-carotene and other compounds. Therefore, the pharma and nutrition industry is heavily interested in the fast and simple extraction of high-quality piperine.
Conventional piperine and piperidine extraction is performed by time-consuming solvent extraction using toxic DMC (dichloromethane). Ultrasonic extraction excels conventional solvent extraction by higher yields, the use of non-toxic solvents (e.g. ethanol) and a rapid extraction process. High-performance ultrasound creates cavitation in liquids. Acoustic or ultrasonic cavitation generates locally extreme conditions such as super-high temperature and pressure differentials, liquid jets and shear forces. These ultrasonic forces break cell walls and increase the mass transfer between cell interior and the surrounding solvent so that the bioactive substances are released. Ultrasonic extraction is a proven technique to isolate targeted compounds such as piperine from ground pepper (piper nigrum, piper longum).

Optimum Extraction Conditions

One of the most important advantages of the ultrasonic isolation is the precise control of all process parameters. Ultrasonic intensity (amplitude, power, duty cycle), extraction time, solvent, solid to solvent ratio, and temperature can be tuned to optimal conditions in order to obtain the highest yield of high-quality piperine.

Ultrasonic extractors such as the UIP1000hdT are used for the extraction of piperine.

UIP1000hdT with ultrasonic flow reactor

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Advantages:

  • higher yield
  • high-quality extracts
  • non-thermal
  • rapid extraction
  • safe process
  • environmental-friendly

Exemplary Protocol for Ultrasonic Piperine Extraction

In a small scale beaker setup, maximum yield of piperine (5.8 mg/g) from ground Piper longum is obtained at optimized ultrasonic extraction conditions, which have been found to be the following:
ultrasonic device UP200St or UP200Ht (200W, 26kHz)
ultrasonic parameters: 100% amplitude, 80% duty cycle
sonication time: approx. 18 min.
solvent: ethanol
solid to solvent ratio: 1:10
temperature: 50°C

Superior Results

UP200Ht - a powerful handheld ultrasonic device.Ultrasonic extraction has significant advantages over traditional batch and solvent extraction. Rathod (2014) shows that the extraction time is reduced from 8h batch solvent extraction and 4h Soxhlet extraction is reduced to 18 min. ultrasonic extraction. Furthermore, ultrasonic extraction gives a higher extraction yield of piperine. Extraction yields of piperine obtained from Soxhlet extraction and batch extraction methods were found to be 1.67 mg/g and 0.98 mg/g, respectively, which were much lower than the ultrasonically obtained yield of 5.8mg/g. Rathod (2014) concludes that the ultrasound-assisted extraction of natural phytoconstituents such as piperine diminishes the problem of low extractability and long extraction times over traditional methods.

Ultrasound is successfully used for the extraction of essential oils from black pepper, too. Click here to learn more about the ultrasonic hydrodistillation of essential oils!

Ultrasonic Extractors

Hielscher Ultrasonics is long-experienced manufacturer of high-performance ultrasonic extraction systems. Our products portfolio ranges from small, powerful lab ultrasonicators to robust bench-top and industrial systems, which deliver high intensity ultrasound for the efficient extraction and isolation of bioactive substances (e.g. piperine, curcumin etc.).
All ultrasonic devices from 200W to 16,000W feature a coloured display for digital control, an integrated SD card for automatic data recording, browser remote control and many more user-friendly features. The sonotrodes and flow cells (the parts, which are in contact with the medium) can be autoclaved and are easy to clean.
All our ultrasonicators are built for 24/7 operation, require low maintenance and are easy and safe to operate.

The table below gives you an indication of the approximate processing capacity of our ultrasonicators:

Batch Volume Flow Rate Recommended Devices
0.5 to 1.5mL n.a. VialTweeter
1 to 500mL 10 to 200mL/min UP100H
10 to 2000mL 20 to 400mL/min UP200Ht, UP400St
0.1 to 20L 0.2 to 4L/min UIP2000hdT
10 to 100L 2 to 10L/min UIP4000
n.a. 10 to 100L/min UIP16000
n.a. larger cluster of UIP16000

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Literature/References

  • Cao X.; Ye X.; Lu Y.; Mo W. (2009): Ionic liquid-based ultrasonic assisted extraction of piperine from white pepper. Analytica Chimica Acta 640, 2009. 47-51.
  • Rathod S.S.; Rathod V.K. (2014): Extraction of piperine from Piper longum using ultrasound. Industrial Crops and Products Vol. 58, 2014. 259-264.


Facts Worth Knowing

Ultrasonic Extraction

Ultrasonic extraction of bioactive substances from botanicals is based on the principle of acoustic cavitation. Acoustic cavitation occurs when highly intense ultrasound waves (e.g. high amplitudes of 100µm, generated by 20-26kHz ultrasound) are coupled into a liquid. The cavitational shear forces perforate and rupture the cell walls of the plant material, and push and pull the surrounding solvent in and out of the cell interior. After the extraction process, the solvent carries the targeted molecules, which can then separated (e.g. by centrifugation). Ultrasonic extraction is well known to give high yields of intact phyto extracts.

Ultrasonic disruptors are used for extractions from plant materials

Ultrasonic extraction from cells: the microscopic transverse section (TS) of apical stem of mint (Mentha piperita) shows the mechanism of actions during ultrasonic extraction from cells (magnification 2000x) [resource: Vilkhu et al. 2011]

Piperine

Piperine (1-piperyol-piperidine) is the main pungent compound of pepper (piper nigrum / piper longum, Piperaceae). Pepper flavour, its pungency, and thus its quality, are correlated with the piperine amount. This quality attribute can be changed by hydrolysing piperine, so that the piperidine ring is cleavaged.
Piperine is known for various pharmacological effects, e.g. antifungal, antidiarrhoeal, anti-inflammatory, and 5-lipoxygenase and cyclooxygenase-1 inhibitory activities. Furthermore, piperine increases the bioavailability of curcumin by 2000%. Therefore, piperine is a popular substance used in supplement formulations (e.g. BioPerine®).
Piperine can be extracted from Piper nigrum and Piper longum.
Piperidine is a cyclic secondary amine, which is a molecular structure found in many plant alkaloids. Piperidine results from hydrolysis of piperine. Piperidine and its derivatives are ubiquitous building blocks in the synthesis of pharmaceuticals and fine chemicals.

Pepper

Piper nigrum, black pepper, is a flowering vine in the family Piperaceae. It is cultivated for its peppercorn fruits which are usually dried and used as a spice and seasoning. Black, green and white peppercorns are all obtained from the black pepper plant. The different colors are the result of the treatment and preparation of the peppercorns. Black peppercorns are obtained by boiling the unripe drupes in hot water and dry them afterwards. White pepper is harvested as fully ripe berries of the pepper plant; then the dark skin of the ripe fruit removed (retting). Green peppercorns are made from the unripe drupes by treating them with sulphur dioxide, canning or freeze-drying in order to retain its green colorants.

Piper longum Linn, also known as Indian long pepper (pipli), is a close relative to Piper nigrum and has a taste similar, but hotter taste than Piper nigrum.
The fruits of Piper longum contains approx. 1% volatile oils, resin, alkaloids piperine and piperlonguminine, a waxy alkaloid Nisobutyldeca-trans-2-trans-4-dienamide and a terpenoid substance. The piperidine alkaloid piperine is responsible for the spicy, pungent taste of pepper berries. Piperlongumine is a pharmacological active substance which shows activity against many cancers including prostate, breast, lung, colon, lymphoma, leukemia, primary brain tumors and gastric cancer.
Furthermore, the following amounts of minerals can be found in pepper berries: 1230mg/100g calcium, 190mg/100g phosphorous, and 62.1mg/100g iron. The roots contain piperine, piperlongumine or piplartine and dihydrostigmasterol.