Determination of oxalic acid content in hydrochloric acid samples was accomplished using HPLC. LC-20AD Prominence chromatograph (Shimadzu Co. Ltd., Kyoto, Japan) was used. The analysis was conducted on a Shodex 1C SI-90 4E column (4.0 mm Ø × 250 mm, Shodex Group, Tokyo, Japan). Detection was performed using diode array detector SPD-M20A at 210 nm. The column thermostat temperature was 33 °C, isocratic flow (1.5 mL·min−1): 1.7 mM NaHCO3 + 1.8 mM Na2CO3. Retention time for oxalate anion using this method is 28.2 ± 0.2 min.
Lc 20ad prominence chromatograph
Manufactured by Shimadzu
Sourced in Japan
The LC-20AD Prominence chromatograph is a high-performance liquid chromatography (HPLC) system manufactured by Shimadzu. It is designed to perform precise and reliable liquid chromatography analysis. The LC-20AD Prominence provides accurate and reproducible results for a wide range of analytical applications.
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Lab products found in correlation
Multiquant 2, by AB Sciex (2 mentions)
Analyst 1, by AB Sciex (2 mentions)
Qtrap 6500 mass spectrometer, by AB Sciex (1 mentions)
Cyclone plus storage phosphor system, by PerkinElmer (1 mentions)
Trifluoroacetic acid hplc grade, by Merck Group (1 mentions)
Absciex 6500 qtrap mass spectrometer, by AB Sciex (1 mentions)
4 protocols using lc 20ad prominence chromatograph
1
Oxalic Acid Determination in HCl via HPLC
2
HPLC-MS/MS Quantification Protocol
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HPLC-MS/MS analyses were performed using a Shimadzu LC-20AD Prominence chromatograph equipped with a SIL-20AC cooled autosampler and a gradient pump. A column filled with a reversed-phase ProntoSil 120-AQ C18 sorbent (Econova, Novosibirsk, Russia) was used. Water with 0.1% HCOOH was used as the mobile phase A, and ACN containing 0.1% HCOOH was used as the mobile phase B. The gradient was as follows: 0 min—5% B; 1 min—5% B; 2 min—95% B; 5 min—100% B; the flow rate was 300 μL/min; the injection volume was 10 μL. The column was then equilibrated for the next analysis.
Mass spectrometric detection was carried out on a 6500 QTRAP mass spectrometer (SCIEX, Framingham, MA, USA) using electrospray ionization. The following conditions were used: positive MRM mode, CUR (curtain gas) = 30 psi, CAD (collision-activated dissociation gas) = High, IS (ion source voltage) = 5500 V, TEM (temperature) = 350 °C, GS1 (sprayer gas) = 20 psi, GS2 (evaporator gas) = 20 psi, dwell time = 100 msec. The instrument was controlled, and information was collected using Analyst 1.6.3 software (AB SCIEX), chromatograms were processed using MultiQuant 2.1 software (AB SCIEX, Framingham, MA, USA).
Mass spectrometric detection was carried out on a 6500 QTRAP mass spectrometer (SCIEX, Framingham, MA, USA) using electrospray ionization. The following conditions were used: positive MRM mode, CUR (curtain gas) = 30 psi, CAD (collision-activated dissociation gas) = High, IS (ion source voltage) = 5500 V, TEM (temperature) = 350 °C, GS1 (sprayer gas) = 20 psi, GS2 (evaporator gas) = 20 psi, dwell time = 100 msec. The instrument was controlled, and information was collected using Analyst 1.6.3 software (AB SCIEX), chromatograms were processed using MultiQuant 2.1 software (AB SCIEX, Framingham, MA, USA).
3
Radiochemical Analysis of [177Lu]Lu-PSMA-617
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Several radio-TLC methods were used to analyze the radiochemical conversion and radiochemical purity of [177Lu]Lu-PSMA-617 preparations. The main TLC methods used are listed in Table 1 .
Radiography of the TLC-strips was performed using a miniGita radio-TLC scanner (Elysia-Raytest, Straubenhardt, Germany) as well as a Cyclone® Plus storage phosphor system (PerkinElmer, Waltham, MA, USA).
HPLC analysis of the [177Lu]Lu-PSMA-617 preparations was carried out using an LC-20AD Prominence chromatograph (Shimadzu Co., Ltd., Kyoto, Japan) equipped with a diode array detector SPD-M20A and a MiniScanPRO TLC/HPLC Flow-Count system (Eckert & Ziegler Eurotope GmbH, Berlin, Germany) with FC-3200 NaI/PMT and FC-3600 Plastic Scintillator/PMT-based detectors (⌀0.25 × 5 mm flow cell (PEEK tubing). Three different methods were used in this study—Table 2 . The reversed phase C18 columns were purchased from Phenomenex® (Torrance, CA, USA). In all three methods, solvent A was 0.1% (v/v) TFA in water (TFA—trifluoroacetic acid HPLC grade Sigma-Aldrich/Merck (St. Louis, MO, USA)).
Radiography of the TLC-strips was performed using a miniGita radio-TLC scanner (Elysia-Raytest, Straubenhardt, Germany) as well as a Cyclone® Plus storage phosphor system (PerkinElmer, Waltham, MA, USA).
HPLC analysis of the [177Lu]Lu-PSMA-617 preparations was carried out using an LC-20AD Prominence chromatograph (Shimadzu Co., Ltd., Kyoto, Japan) equipped with a diode array detector SPD-M20A and a MiniScanPRO TLC/HPLC Flow-Count system (Eckert & Ziegler Eurotope GmbH, Berlin, Germany) with FC-3200 NaI/PMT and FC-3600 Plastic Scintillator/PMT-based detectors (⌀0.25 × 5 mm flow cell (PEEK tubing). Three different methods were used in this study—
4
LC-MS/MS Quantification of Compounds 4c and 5d
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Analyses were carried out using a Shimadzu LC-20AD Prominence chromatograph (Shimadzu, Tokyo, Japan) equipped with a binary gradient pump, cooled autosampler SIL-20AC and column oven. A column packed with a reversed-phase sorbent ProntoSil 120-AQC18 (2 × 75 mm, 5 µm, EcoNova, Novosibirsk, Russia) was used for chromatographic separations. Mobile phase was water (eluent A) and MeOH (eluent B). The following gradient was used: 0 min—10% B; 1 min—90% B; 4.6 min—90%; 4.7 min—100% B; 6.0 min—100% B, followed by the equilibration of the column. Flow rate was 330 µL/min; injection volume was 10 µL. Mass spectrometric detection was performed on an ABSCIEX 6500 QTRAP mass spectrometer (AB SCIEX, Framingham, MA, USA) using negative electrospray ionization. The following parameters were set for the detection: scan mode—MRM, curtain gas (CUR) = 30 psi, collision-induced dissociation gas (CAD) = Medium, ion source voltage (IS) = 5500 V, gas drier temperature (TEM) = 250 °C, sprayer gas (GS1) = 15 psi, drier gas (GS2) = 20 psi, entrance potential (EP) = 10 V and dwell time = 80 msec. Detection parameters for agents 4c and 5d are shown in Table S1 (Supporting Information) . The instruments were controlled, and the data were collected using Analyst 1.6.3 software (AB SCIEX); data processing was performed using MultiQuant 2.1 software (AB SCIEX).
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