Methods of solid phase extraction. Methods of solid phase extraction

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Handling of columns For elution either apply pressure at the top of the column or apply vacuum at the column end. For this purpose several procedures are possible as shown in the adjacent figures. The adaptor shown in fig. a) can be used for coupling of several columns of the same or different sizes. a) With the aid of a disposable syringe and an adaptor the eluent can be pressed through the column. b) For drawing the eluent through a column it can be placed on an aspirator bottle by means of a syringe needle, or it can be used on the vacuum manifold described below. columns can be used with all vacuum systems with Luer fitting. c) The same result can be obtained by using the column in a centrifuge tube. Handling of CHROMAFIX cartridges With the aid of a syringe the required solvents for conditioning, washing and elution as well as the sample itself can be easily pushed through the adsorbent without high pressures. Of course, CHROMAFIX cartridges can be used with vacuum manifolds, the Luer tip of the cartridges fits directly into the Luer fittings of the vacuum manifold. Handling of large sample volumes For larger sample volumes MACHEREY-NAGEL has developed the LV columns, which are available with three different adsorbent weights (100, 200 and 500 mg) and feature a funnel-shaped reservoir of 15 ml volume. If very large sample volumes are to be extracted, we recommend the tubing adaptors, which consist of an adaptor for columns and 1 m coloured Teflon tubing with weight. The package contains 4 adaptors with tubes of different colours. Application of the tubing adaptor a) Use with a disposable syringe disposable syringe adaptor CHROMAFIX cartridge column syringe needle vacuum reservoir b) Use with vacuum flask or or manifold Teflon tube column CHROMAFIX cartridge c) Use of in a centrifuge column centrifuge tube 226

vacuum manifolds for simultaneous preparation of up to 12, 16 or 24 samples If several samples are to be treated simultaneously, we recommend our vacuum manifolds. 2 4 7 9 8 There are several possibilities for applying different sample volumes. Small samples can be applied directly to the column. For medium size samples we have developed our LV columns (7) with 15 ml sample reservoir. Especially for this column type we offer a vacuum manifold with 16 positions, because with the manifold for 24 columns only every second position can be used. Alternatively, you may use the polypropylene sample reservoirs (30 or 70 ml) from our programme of SPE accessories, which can be fitted onto the column with the aid of an adaptor (8). Sample reservoirs fit directly onto the upper Luer fitting of the CHROMAFIX cartridges. For large sample volumes we recommend our tubing adaptors (9), which fit onto the columns. The other end of the tubing is placed into the sample, which, by applying vacuum, is continuously drawn into the column. For special applications, which require maximum protection from cross contamination we supply chrome-plated brass valves and stainless steel connectors, the application of which is shown in figure 2. These special stainless steel needles are fitted through the lid; thus the sample only has contact with the inert needle and can flow directly into the receptacle. SPE column 1 Figure 1: vacuum manifold for up to 24 columns We supply such manifolds (figure 1) for up to 12, 16 or 24 columns or CHROMAFIX cartridges, respectively. The manifolds consist of rectangular glass cabinets (1) with vacuum gauge (3) and a polypropylene lid (2), which can hold the columns or cartridges. The replaceable valves (4) on the lid allow individual vacuum control for each solid phase extraction column, if required. The cabinet is fitted with a variable rack (5) with exchangeable partitions, which accept a wide variety of vessels like test tubes, measuring flasks, scintillation vials, autosampler vials, plastic vials and many more. With the control valve (6) the vacuum in the chamber can be adjusted and read from the gauge. 5 3 6 frit solid phase frit Luer fitting, female lid of vacuum manifold with bore Luer fitting, male stainless steel needle connector Figure 2: cross-contamination-free elution with stainless steel or PTFE connectors (right) compared to the standard configuration (left) 227

If the eluate has to be evaporated, this can be performed with the so-called drying attachment (10, see figure 3). This special lid has a gas connector on one side (11), from which the gas is fed simultaneously to the 12 or 24 stations (12). Thus 12 or 24 eluates can be evaporated simultaneously by just changing the lid and applying a stream of inert gas, e.g. nitrogen. 10 12 11 Figure 3: vacuum manifold with drying attachment Handling of MULTI 96 The MULTI 96 are particlularly designed for the use in all common robotic workstations or commercially available liquid handling systems. Alternatively, the use of multi-channel pipettors facilitates a manual liquid transfer. The extraction is carried our using the MULTI 96 vacuum manifold. With the help of the control valve the vacuum of the manifold can be adjusted leading to an optimum flow rate through the MULTI 96 SPE plate. A reservoir tank and 96-well collection plates (96 x 0.5 or 96 x 2 ml) made of polypropylene can be supplied as accessories. An interesting alternative for collection of the eluates is a collection rack, which can be fitted with twelve 8-well strips of polypropylene tubes (each 1 ml). If you have to work on less than 96 samples, you can seal individual rows of the 96-well plate with a PTFE-covered rubber pad. 228

Accessories for solid phase extraction Description Pack of Cat. No. vacuum manifold and replacement parts Vacuum manifold complete consists of: glass cabinet with lid and lid gasket, removable needles on 1 730150 lower side of lid, vacuum gauge, control valve, valves and caps, variable rack, for 12 columns Vacuum manifold as described above, for 16 LV columns 1 730360 Vacuum manifold as described above, for 24 columns 1 730151 Glass cabinet without accessories, for 12 columns 1 730173 Glass cabinet without accessories, for 16 LV or 24 columns 1 730174 PP tanks for vacuum manifold for 12 columns 2 730233 Lid with gasket, for 12 columns, including Luer fittings and valves 1 730175 Lid with gasket, for 16 LV columns, including Luer fittings and valves 1 730365 Lid with gasket, for 24 columns, including Luer fittings and valves 1 730176 Gaskets for lid, for 12 columns 2 730177 Gaskets for lid, for 24 columns 2 730178 Luer stoppers for vacuum manifold, white 12 730194 Luer fitting for lid, female Luer fittings as above 1 730183 12 730183.12 Luer fitting for lid, male Luer fittings as above 1 730184 12 730184.12 Drying attachment, for 12 columns 1 730187 Drying attachment, for 24 columns 1 730188 Collecting rack for 12 columns 1 730157 Collecting rack for 16 LV columns 1 730366 Collecting rack for 24 columns 1 730153 Vacuum gauge, complete with accessories 1 730179 Stainless steel needles 12 730152 Polypropylene needles 12 730154 Valves, plastic 12 730185 Valve, brass, tarnished 1 730189.1 Valves, brass, tarnished 12 730189.12 Stainless steel connectors 12 730106 PTFE connectors 12 730564 PTFE connectors with valve 12 730563 Tubing adaptors for application of large sample volumes to 1, 3 and 6 ml glass columns 4 730387 Tubing adaptors for application of large sample volumes to 1, 3 and 6 ml 4 730243 Tubing adaptors for application of large sample volumes to 15, 45 and 70 ml 4 730386 MULTI 96 accessories for SPE 96-well plates MULTI 96 vaccum manifold with reservoir tank, vacuum gauge, and control valve 1 738630.M 96-well microtiter plates (polypropylene) 96 x 0.25 ml 10 738651 96-deep-well collecting plate (polypropylene) 96 x 2 ml 1 738650 Collection racks with polypropylene tube strips (twelve 8-well strips) 96 x 1.0 ml 5 738637 Polypropylene tube strips (twelve 8-well strips) 96 x 1.0 ml 10 738652 8-well strip sealing caps for PP tube strips (Cat. No. 738652) 30 738638 Reservoir tanks (polypropylene) 2 738639.M Butyl rubber pad, PTFE covered, 125 x 85 mm 1 738645 For MULTI-96 filter plates see page 245 229

Accessories for solid phase extraction Description Pack of Cat. No. empty columns and accessories Empty glass columns with glass fibre frits, 1 ml 100 730170 Empty glass columns with glass fibre frits, 3 ml 50 730171 Empty glass columns with glass fibre frits, 6 ml 30 730172 Glass fibre frits for glass columns 1 ml 250 730190 Glass fibre frits for glass columns 3 ml 250 730191 Glass fibre frits for glass columns 6 ml 250 730192 Empty with PE frits, 1 ml 100 730159 Empty with PE frits, 3 ml 50 730160 Empty with PE frits, 6 ml 30 730161 Empty with PE frits, 15 ml one filter element is already inserted 20 730230 Empty with PE frits, 30 ml in the polypropylene column 20 730380 Empty with PE frits, 45 ml 20 730355 Empty with PE frits, 70 ml 20 730158 Empty with PE frits, 150 ml 20 730474 PE frits for 1 ml 250 730164 PE frits for 3 ml 250 730162 PE frits for 6 ml 250 730163 PE frits for 15 ml 250 730351 PE frits for 30 ml 250 730034 PE frits for 45 ml 250 730356 PE frits for 70 ml 250 730026 PE frits for 150 ml 250 730475 Empty LV with PE frits, 15 ml, for 100 mg sorbent weight 50 732500 Empty LV with PE frits, 15 ml, for 200/500 mg sorbent weight 50 732501 PE frits for LV 15 ml for 100 mg sorbent weight 250 732019 PE frits for LV 15 ml for 200/500 mg sorbent weight 250 732020 Adaptor (PVDF) for glass columns (1, 3 and 6 ml) 1 730104 Adaptors as above 10 730105 Adaptor (PP) for (1, 3 and 6 ml) 1 730100 Adaptors as above 10 730101 Adaptor (PE) for (15, 45, 70 ml) 1 730350 Adaptors as above 10 730385 Adaptor (PE) for (30 and 70 ml) 1 730566 Reservoir column 30 ml, polypropylene, with one adaptor for 1, 3, 6 ml 1 730102 10 Reservoir columns 30 ml with one adaptor for 1, 3, 6 ml 1 kit 730103 Reservoir column 70 ml, polypropylene, with one adaptor for 1, 3, 6 ml 1 730381 10 Reservoir columns 70 ml with one adaptor for 1, 3, 6 ml 1 kit 730382 Reservoir column 70 ml, polypropylene, with one adaptor for 15, 45, 70 ml 1 730388 10 Reservoir columns 70 ml with one adaptor for 15, 45, 70 ml polypropylene columns 1 kit 730389 230