SiliaMetS® Metal Scavengers Leaching & Stability Studies
Now that our SiliaMetS Metal Scavengers are being used by many pharmaceutical and biotechnological companies, each SiliaMetS manufactured by SiliCycle is submitted to an extensive washing procedure which ensures a product with extremely low levels of extractables and leachables.
SiliCycle has implemented a quality control procedure regarding possible leaching that includes loading and reactivity determination, as well as leachables and extractables analysis (silica gel purity ≥ 99.995%). The solution must be free of contaminants for the product to successfully pass the rigorous quality control tests.
To address the end users concerns for potential leaching of impurities into reaction mixtures using SiliaMetS, we have performed three typical metal containing reactions. We then investigated the detection, identification, and quantification of possible impurities resulting from the scavengers used.
Transition metal catalyzed reactions performed
The following three transition metal catalyzed reactions were performed:
Experimental Procedure
Crude reaction mixtures (8 mL) were placed in a standard polypropylene tube equipped with a 20 µm frit and filled with 1 g of the appropriate SiliaMetS Metal Scavenger and mixed for 4 h at either room temperature or 80°C. Solutions were then filtered through a 0.02 µm filter prior to analysis.
Leaching Analysis
For each SiliaMetS, silanes leaching was analyzed by ICP-OES which has proven to be very sensitive for silicon quantification (detection limit in solution is 0.125 ppm). Traces of non-silicon containing impurities were also analyzed by GC-MS and 1H NMR Analysis. Only results for SiliaMetS Thiol and DMT are shown. However, no evidence of any impurities was found for allSiliaMetS. Contact us to get the complete study.
Gel Purity Calculation Example
Silanes Leaching Analysis by ICP-OES
Results shown in the table below for SiliaMetS Thiol & DMT confirm that minimal leaching occurs with SiliCycle SiliaMetS.
Note: concentration given are in ppm and represent mg of silicon leached per kg of SiliaMetS.
| Stability of SiliaMetS in Suzuki, Stille and Ring-Closing Metathesis reactions | |||||
| Reaction (solvent) | Temperature | SiliaMetS Thiol | SiliaMetS DMT | ||
| [Silicon] | Gel Purity | [Silicon] | Gel Purity | ||
| Suzuki (Toluene) | 22°C | 2 ppm | 99.9998 % | 1 ppm | 99.9999 % |
| 80°C | 2 ppm | 99.9998 % | 2 ppm | 99.9998 % | |
| Stille (1,4-Dioxane) | 22°C | 2 ppm | 99.9998 % | 1 ppm | 99.9999 % |
| 80°C | 1 ppm | 99.9999 % | 3 ppm | 99.9997 % | |
| Ring-Closing Met (DCM) | 22°C | 2 ppm | 99.9998 % | 2 ppm | 99.9998 % |
| Note: Very low levels of silicon were detected in most experiments, giving products purity higher than 99.995 %. | |||||
Non-Silicon Leaching Analysis
| Gas chromatography-mass spectrometry (GC-MS) | 1H NMR Analysis (d6-dmso) |
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Compared to the silica blank spectrum (bare silica in solvent), neither experiment showed evidence of any impurities for either SiliaMetS Thiol or DMT.
Note: each experiment was ran on a 1 g aliquote of SiliaMetS and was shaken for one hour at room temperature. In GC-MS spectrum, peak at 8.5 minutes is the internal standard (1-fluoronaphthalene, 100 ppm). In NMR spectrum, peaks at 2.4 and 3.4 ppm are, respectively, d6-dmso and water contained in deuterated solvent.
Stability Study (Shelf Life)
| SiliCycle certifies that SiliaMetS Metal Scavengers stored under recommended conditions in an undamaged container are guaranteed to perform for over two years from the manufacturing date without loss of performance, prouved by results at right. |
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13 Item(s)
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SiliaBond® Amine
SiliaBond® Amine (Si-NH2) is an effective scavenger of acid chlorides, sulfonyl chlorides, isocyanates and other electrophiles. Si-NH2 has been shown to be effective metal scavenger and catalyst for Knoevenagel reactions. SiliaBond Amine is also used in chromatography as normal phase sorbent.
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SiliaMetS® Diamine
SiliaMetS® Diamine (Si-DIA) is a proven scavenger for metals and electrophiles. It scavenges acids, acid chlorides, anhydrides, aldehydes, isocyanates, and chloroformates as well as Pb, Ni, and Cd.
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SiliaSep™ Flash Cartridges Amine
Good alternative for normal phase purification of compounds with basic properties, which would normally have to be purified by reversed-phase.
SiliaSep flash amine cartridges offer a superior alternative to the other cartridges available on the market.
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SiliaSep™ Flash Cartridges Triamine
SiliaSep flash triamine cartridges offer a superior alternative to the other cartridges available on the market.
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SiliaSep™ Flash Cartridges Diamine
SiliaSep flash diamine cartridges offer a superior alternative to the other cartridges available on the market.
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SiliaSep™ Flash Cartridges - Open Top (OT) Amine
SiliaSep™ OT flash cartridges are compatible with FlashMaster instrument.
Good alternative for normal phase purification of compounds with basic properties, which would normally have to be purified by reversed-phase.
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SiliaSep™ Flash Cartridges - Biotage™ Compatible (BT) Amine
SiliaSep™ BT flash cartridges are compatible with Biotage i-style compression modules.
Good alternative for normal phase purification of compounds with basic properties, which would normally have to be purified by reversed-phase.
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SiliaSep™ Flash Cartridges - Büchi™ Compatible (BU) Amine
SiliaSep™ BU flash cartridges are compatible with Büchi Sepacor flash chromatography instrument.
Good alternative for normal phase purification of compounds with basic properties, which would normally have to be purified by reversed-phase.
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SiliaPrep™ SPE Cartridges Amine (WAX)
SiliaPrep Amine is a weak anion exchanger sorbent used in replacement of SAX for strong anions to avoid irreversible retention. Can also be employed as a metal scavenger and norman phase conditions.
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SiliaPrep™ SPE Cartridges Amine nec (WAX)
SiliaPrep Amine nec is a weak anion exchanger sorbent used in replacement of SAX for strong anions to avoid irreversible retention. Can also be employed as a metal scavenger and norman phase conditions.
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SiliaPrep™ SPE Cartridges Diamine
SiliaPrep diamine can be used in replacement of SAX for strong anions to be irreversible retention. Can also be employed as metal scavenger and in normal-phase conditions.
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SiliaPrep™ SPE Cartridges Diamine nec
SiliaPrep diamine can be used in replacement of SAX for strong anions to be irreversible retention. Can also be employed as metal scavenger and in normal-phase conditions.
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SiliaPrep™ SPE Cartridges Triamine
SiliaPrep Metal Scavengers will lower the residual metal concentration of various metal complexes to single digit ppm.
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- Metal to Remove
- Family / Formats
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- 60 Å (13)
- Endcapping
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- Endcapped (13)
- Non-endcapped (1)
- Cartridges Volume
- Bed Weight
- Particle Size
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