13 Table 1. Results of experiments done with Rocket Evaporation System and SampleGenie
Test No
Fraction Composition
Volume (mls)
R1396 100 R1396 100 R1396 100 R1424 100 R1424 100 R1397 100 R1397 100 R1397 100 R1432 100 R1432 100 R1389 100 R1432 100 R1432 100 R1424 100 R1424 100 R1384 100 R1384 100 R1419 200 R1419 200 R1246 200 R1246 200 R1426 200 R1426 200 R1432 200 R1432 200 R1369 200 R1405 200
MeCN %
20 20 20 30 30 40 40 40 50 50 60 60 60 70 70 80 80 20 20 20 20 40 40 50 60 70 80
H2O %
80 80 80 70 70 60 60 60 50 50 40 40 40 30 30 20 20 80 80 80 80 60 60 50 40 30 20
Dioxane addition (mls)
0
10 20 0
Recovery
% End mass
Start mass
98.9 0.1049 0.1037 97.7 0.1024 0.1 99.6 0.1076 0.1072 99.7 0.1016 0.1013
20 100.2 0.1048 0.105 0
20 30
100.3 0.1057 0.106 99.1 0.1037 0.1028 93.5 0.1021 0.0955
Caffeine Caffeine Caffeine Caffeine Caffeine Caffeine Caffeine Caffeine
40 100.3 0.1015 0.1018 Cimetidine 20 105.4 0.1004 0.1058 Cimetidine 30
Test
90 80 70 60 50 40 30 20 10
Fraction Volume
100ml -
15-30 20-30 20-30 20
0-20 0-20 0-20 -
200ml -
30-50 50 50 50
0-20 0-20 0-20 -
Figure 5. Look up table of 1,4-dioxane addition for fraction handling Conclusion 97.6 0.1046 0.1021 Hydrocortisone
20 103.2 0.1009 0.1041 Cimetidine 30 104.7 0.105 0.1099 Cimetidine 20
99.2 0.1092 0.1083 Hydrocortisone
30 102.0 0.1022 0.1042 Hydrocortisone 0 5
30 106.1 0.2051 0.2177 20 102.4 0.1945 0.1991 0
20 101.2 0.1082 0.1095 0
20 50
101.3 0.1023 0.1036 Hydrocortisone 99.3 0.1052 0.1045 Hydrocortisone Caffeine Caffeine Caffeine Caffeine Caffeine Caffeine
98.7 0.1028 0.1015
101.9 0.104 0.106 99.8 0.1065 0.1063
99.2 0.1962 0.1946 Cimetidine
50 108.2 0.1946 0.2105 Cimetidine 50 50
88.3 0.1059 0.0935 Hydrocortisone 95.8 0.1921 0.184 Hydrocortisone
SampleGenie is a straightforward way to concentrate or dry large volume samples directly into smaller vials using the revolutionary Rocket evaporation system. To overcome the potential problem of dissolved samples crashing out of solution, sticking to the glass fl ask, and therefore not getting into the vial, the addition of a moderate quantity of 1,4-dioxane is a simple and effective method. This work has been summarised in a look up table to assist users determine how much 1,4-dioxane is required to add for different fractions.
References
1. Evaluation of a new technology which enables large volumes to be concentrated directly into a small vial for use in environmental analysis. Dr. Raffaele Faita & Dr. Agostino Brunetta, Leochimica Laboratories, Italy.
First published in International Environmental Technology 2008 Vol. 18 No. 6 pp44 & 45,
2. Development of a Novel Parallel Evaporator - Developing high power condensation heating to enable very fast parallel evaporation, in a safe, and controlled manner. Roger Lee-Smith & David Griffi n Genevac Ltd, Ipswich, UK.
First published in LabMate October 2008.
3. Assessment of Sample Recovery using SampleGenie to Automate Fraction Pooling into a Storage Vial, Peter Bennett, Servier Research, Slough, UK.
4. Evaluation of a Novel, Large Volume Evaporative Sample Preparation Technique. Felix Massat, Benoît Planel, & Antoine Venezia, Laboratoire départemental d’analyses de la Drôme, Valence, France.
Acknowledgements Tefl on is a registered trade mark of E. I. du Pont de Nemours and Company
Read, Share and Comment on this Article, visit:
www.labmate-online.com/article Silica-Free Centrifugal Partition Chromatography (CPC) Columns Released
Gilson have announced an extension to its PLC purifi cation system offering by introducing centrifugal partition chromatography (CPC) columns, available with a wide range of reusable, silica-free column possibilities. CPC columns coupled with a PLC Purifi cation System offer improved yields and better cost effi ciencies over fl ash chromatography and preparative HPLC techniques. The easily scalable systems are ideal for natural compound purifi cation, natural extract fractionation, and general molecule purifi cations for cosmetics, food supplements, and pharmaceuticals. Using Gilson’s CPC technology in the natural product purifi cation process results in greater than 95% recoveries with 99% purity. The CPC columns are ideal for labs that are going green. They create less waste by being reusable, and provide cost savings by eliminating expensive column replacement and silica recycling. The technology also uses fi ve times less solvent than preparative HPLC and fl ash chromatography.
The silica-free CPC columns offer large injection capacity, from milligrams to multi-kilograms depending on the size of CPC column. Gilson purifi cation systems provide preparative- to industrial-scale purifi cation of highly complex samples without sample pretreatment. To streamline workfl ows, this Gilson purifi cation system can be completely controlled through Gilson Glider software. As chromatographic columns, the Gilson CPC can connect to any preparative liquid chromatography system. Gilson offers complete purifi cation solutions. Now with the combination of Gilson’s CPC column with the PLC Purifi cation Systems, researchers have the fl exibility to easily use either CPC, fl ash, or preparative HPLC columns as needed.
For more information on Gilson CPC or to download technical notes about CPC, visit
gilson.com.
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Topics Announced for Symposium on Hyphenated Techniques
The organisers of the 15th International Symposium on Hyphenated Techniques in Chromatography and Separation Technology (HTC-15) have announced the conference themes for their next event. Anyone wishing to present a Paper or Poster may submit an abstract via
www.ilmexhibitions.com/htc. Early bird registration is also now available from the website.
Taking place at Cardiff City Hall from 24th to 26th January 2018, the presentations at HTC-15 will cover issues such as Big Data, sample preparation, separation science, green separations, clinical hyphenations, interfacing and ionisation, ion mobility - mass spectrometry (BMSS), metrology, data handling, microfl uidics and many more. The speakers will address a wide variety of applications including energy, petroleomics, pharma, forensics, the environment, toxicology, drugs in sport, food and beverages.
The HTC events cover all fundamental aspects, instrumental developments and applications of hyphenated techniques. Over the three days of the conference there will be three parallel session, including one dedicated to early career researchers. In addition to the core scientifi c programme, the symposium will host a technical exhibition at which instrumentation manufacturers and developers will present their latest technologies, software and applications related to the hyphenation of separation, detection and sample preparation. There will also be a number of poster presentations and technical seminars.
“With its rich history of successful meetings since 1990, HTC has delivered presentations from internationally renowned experts both from Industry and Academia and this upcoming event will be further enhanced through joint chairing of the Scientifi c Committee by Tom Lynch and Peter Schoenmakers,” says HTC-15 Chair Professor John Langley.
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Fraction % Organic
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