Shimadzu HPLC system

The diastereomeric ratio was determined by Shimadzu HPLC system through Phenomenex Luna Cig (5 micron, 4.60 x 250 mm) column with a flow rate of 1 mL/min and isocratic 80 % MeOH in H2O using SPD-20A UV/VIS detector (230 nm, 254 nm). The 1 1 mixture of (175)- and (17R)-alcohols was prepared by Dess-Martin oxidation of the crude alcohol 2.213 and DIBAL-H reduction of the resulting ketone. 

High Performance Liquid Chromatographic (HPLC) Analysis. A Waters HPLC system (two Waters 501 pumps, automated gradient controller, 712 WISP, and 745 Data module) with a Shimadzu RF-535 fluorescence detector or a Waters 484 UV detector, and a 0.5 pm filter and a Rainin 30 x 4.6 mm Spheri-5 RP-18 guard column followed by a Waters 30 x 3.9 cm (10 pm particle size) p-Bondapak C18 column was used. The mobile phase consisted of a 45% aqueous solution (composed of 0.25% triethylamine, 0.9% phosphoric acid, and 0.01% sodium octyl sulfate) and 55% methanol for prazosin analysis or 40% aqueous solution and 60% methanol for naltrexone. The flow rate was 1.0 mL/min. Prazosin was measured by a fluorescence detector at 384 nm after excitation at 340 nm (8) and in vitro release samples of naltrexone were analyzed by UV detection at 254 nm. 

A representative example of this process is shown in Fig. 2. The spectra of the analyte peaks can be measured at the upslope, the top, and at the downslope, or the whole spectrum of the chromatography peak can be compared. In the latter case, the term totalpeak purity is used, and a purity curve of the peak can also be recorded. These operations can be performed by a HPLC system equipped with a DAD detector [13], or for TLC a densitometer that can measure the UV-Vis spectrum of the analyte spot should be used. If the value of the purity is 0.000 0.8900, it is not pure, and a purity of 0.9000-0.9500 means that the peak is contaminated (Shimadzu Class-VP, Chromatography Data System). 

Using the Tomtec Quadra 96 workstation, 0.1 mL of the ethyl acetate layer was transferred to a 96-well collection plate containing 0.4 mL of acetonitrile in each sample well. The solution was mixed 10 times by aspiration and dispersion on the Tomtec. The plate was then covered with a sealing mat and stored at 2 to 8°C until LC/MS/MS analysis. The HILIC-MS/MS system consisted of a Shimadzu 10ADVP HPLC system and Perkin Elmer Sciex API 3000 and 4000 tandem mass spectrometers operating in the positive ESI mode. The analytical column was Betasil silica (5 fim, 50 x 3 mm) and a mobile phase of acetonitrile water formic acid with a linear gradient elution from 95 5 0.1 to 73.5 26.5 0.1 was used for 2 min. The flow rate was 1.0 mL/min for the API 3000 and 1.5 mL/min for the API 4000 without any eluent split. The injection volume was 10 jjL and a run time of 2.75 min was employed. 

FIGURE 2 Examples of modular and integrated HPLC systems. Upper row (I to r) modular systems Agilent 1100 Series, Jasco LC-2000 Series Lower row (I to r) integrated systems Waters Alliance, Shimadzu LC-2010. 

Acrylate, propionate and acetate were separated by HPLC on a Benson carbohydrate column (30 cm by 0.6 cm i.d.) (Cnromtec, Fort Worth, FL). The HPLC system used a Waters UK6 injector and a Waters Model 6000A pump (Waters Associates, Milford, MA) with a Conductomonitor III Detector (Laboratory Data Control, Riviera Beach, FL) and a Shimadzu Data Processor. The solvent was 0.15 mM H2S04 at a flow rate of 0.5 ml/min. Typical retention times (min) were acrylate, 13.3 acetate, 12.3 propionate, 14.5. The detection limits for acrylate, acetate and propionate were 10, 30 and 40 pM respectively. 

The method recommended by Cooper et al [47] was applied for the analysis of the amino acids Asp, Glu, AAA, Asn, Ser, Tyr, Met, Val, Trp, Phe, lie, Leu and Lys. The HPLC-system consisted of an autosampler with injection valve (Pharmacia Biosystems), pump (Irica), degaser (Gastorr), thermostat (Julabo), precolumn and column (Waters), fluorescence detector (Shimadzu) and a PC (486 DX66)... 

Williams et al. used a high performance liquid chromatographic assay method for dipyridamole monitoring in plasma [71]. The HPLC system uses a Waters model 6000 A solvent delivery pump equipped with a U6K injector, a pBondapak C 9 column (30 cm x 39 mm 10 pm), and a Model 440 absorbance detector. The signal from the detector was quantified using a Shimadzu data processor and an Omni-Scribe recorder. A mobile phase flow rate of 1.5 mL/min was produced by a pressure of approximately 102 atm (1500 p.s.i.). The mobile phase was 50 50 mixture of acetonitrile and 0.01 M sodium phosphate in water (adjusted to pH 7). The absorbance reading of dipyridamole in methanol was made at 280 nm. 

The analyses of aromatic components were performed on a 1525 Binary Waters HPLC with a dual absorbance detector using a Symmetry Cl 8 column and a mobile phase of methanol and water. Carboxylic acids analyses were performed using the same HPLC system with an Atlantis dC18 column and mobile phase. pH was monitored with a Coming 430 pH meter. For most experiments, the total organic carbon was also analyzed using a Shimadzu 5050 TOC analyzer equipped with a NDIR detector coupled with an autosampler ASI 5000. 

The separation of DIB derivatives of morphine and IS were performed using an HPLC system (Shimadzu, Kyoto, Japan) consisting of two pumps (LC-lOATvp) with a system controller (PX-8010), a recorder (FBR-2), a FL detector (RF-550) set at Xex=355 nm and Xem=486 nm, and a Rheodyne 7125 injector (Cotati, CA, USA) with a 20-pL sample loop. In plasma analysis, the mobile phases used were a mixture of acetonitrile-0.1 M acetate buffer (pH5.4) (50 50, v/v, MPl) with a flow rate of 1.0 mL/min and acetonitrile (MP2). The separation program was set as follows the flow rate of MP2 was set at 0 mL/min from 0 to 29 min, rapidly... 

The HPLC system consisted of five LC-lOA pumps, an SIL-lOA auto sample injector, a DGU-14 degasser, a CLD-lOA chemiluminescence detector, an SCL-lOA system controller, a C-R4A integrator, an HIC-6A and a CTO-IOAC column oven (all Shimadzu, Kyoto, Japan). The clean-up colunm (4.6 i.d. X 150 mm), concentrator column (4.6 i.d. X 30 mm), separator colunm (4.6 i.d. X 250 + 150 mm), guard columns 1 (4.6 i.d. X 30 mm) and 2 (4.6 i.d. X 50 mm) were packed with Cosmosil 5C18-MS (Nacalai Tesque, Kyoto, Japan), and the reducer column (4.0 i.d. X 10 mm) was a Nitroarene Reactor Column (Shimadzu). All other conditions were the same as those given in our previous report. ... 

Figure 4.2. Examples of modular and integrated HPLC systems. Modular systems (a) Agilent 1100 Series, (b) Jasco low-pressure mixing system. Integrated systems (c) Waters Alliance, (d) Shimadzu 2010.

Yes (limited to HPLC instruments of Shimadzu, Hitachi, Dionex and Agilent GC 8i HPLC Systems, and Beckman CE)... 

The HPLC system comprised an L-6000 pump (Hitachi, Tokyo, Japan) and an LC-9A pump (Shimadzu, Kyoto, Japan) for deliveries of an eluent and the OPA reagent, a DGU-12A degasser (Shimadzu), a Rheodyne Model 77251 sample injector (Rheodyne, Cotati, CA, USA), aCTO-lOA column oven (Shimadzu), an F-1050 fluorescence detector equipped with a 12 p,l square flow cell, and a D-2500 data processor (Hitachi). Separation was performed at 40°C... 

The tocopherol concentrations in fish samples were determined by the AOCS method (1992). Briefly, extracted TL were dissolved in A2-hexane to a known concentration and injected to the HPLC system equipped with a Shimadzu RF 550 spectrofluorometric detector. The column was a Lichrosorb Si 60 (4 mm id x 250 mm, Merck, Darmstadt, Germany). A mixture of propanol and w-hexane (5 95, v/v) was used as the mobile phase at a flow rate of 1.2 mL/min. Tocopherol concentrations were intrapolated from standard curves. 

Shimadzu Prominence HPLC system with auto sampler, two pumps, and degasser (Lenexa, KS). 

The HPLC-PO-CL system (Fig. 2) consisted of two LC 9A liquid chromatographic pumps (Shimadzu, Kyoto, Japan), a Rheodyne 7125 injector (Cotati, CA, USA) with a 20- tL sample loop, an ultraviolet lamp, Toshiba GL-10 (10 W, 254 nm), a Chemcosorb 5-ODS-UH column (150 x 4.6 mm I.D.), CLD-lOA detector (Shimadzu), a Rikadenki R-61 recorder. PTFE tubing (6.0 m x 0.5 mm I.D., GL Sciences, Tokyo) coiled around the ultraviolet lamp as the on-line for the UV radiation reactor. 

Major manufacturers of HPLC instruments include Waters, Agilent (formerly Hewlett Packard), and Shimadzu, PerkinElmer, Thermo, Beckman, Varian, Hitachi, Jasco, Dionex, Gilson, Scientific Systems (SSI), and Isco. The Internet addresses of these companies can be found in the reference section. HPLC is a mature technology and most manufacturers have highly reliable products with sufficient performance and feature sets to be competitive in the market place. However, there can still be significant differences between the vendors on these performance characteristics on systems (dwell volume, dispersion), pumps (low flow, seal life), autosamplers (carryover, speed, sample capacity, minimum sample volume), and detectors (sensitivity, gradient baseline shift). 

Shimadzu has produced the Prominence HPLC, Agilent has developed the 1200 Rapid Resolution HPLC (Figure 3.22), Thermo Scientific has the Accela LC system and Waters has brought out the Acuity UPLC. Jasco s X-LC system allows two systems to fit in the footprint previously occupied by one traditional system. It is also a modular system of detectors and autosamplers, which allows it to be customised. LC Packings has launched the UltiMate 3000, which is a nanoflow LC system for use with columns of 50 im and larger. Modular systems are common now, e.g. Cecil Instruments produces both HPLC and ion chromatography systems and various detectors can be accommodated including UV-Vis, refractive index, conductivity and fluorescence. 

---