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プレッパーズ 本社

addressShizuoka/Higashi-ku, Hamamatsu-shi/414, Hamamatsu University School of Medicine, Medical Engineering Collaboration Center, 1-20-1 Handayama
phone050-5360-5809
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last updated:Feb 14, 2023
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Application Data: Example of Nucleotide Measurement by TEA Removal

Using the desalting tube "Solnac Tube" for LC/MS! Reduces ionization suppression of nucleotides.

When analyzing highly polar nucleic acids and nucleotides using reversed-phase distribution chromatography, adding ionic species to the eluent can enhance retention by forming neutral ion pairs through ionic bonding. In the case of nucleic acid analysis, it is common to use triethylamine (TEA) as a basic mobile phase for ion pair formation; however, TEA is considered to cause ionization suppression when detecting positive ions due to its excessively high basicity. In this instance, adenylate (AMP) and other samples were used, and TEA in the eluent was removed using a solid-phase extraction tube for positive ion measurement. For details on conditions and analysis results, please download the catalog. 【LC Conditions (Partial)】 ■ Equipment: Waters UPLC H Class ■ Flow rate: 0.3 ml/min ■ Sample: Solutions of AMP, ADP, ATP at 50μM each ■ Injection volume: 10 μL *For more details, please refer to the PDF document or feel free to contact us.

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Application Data: Example of LC/MS Measurement by Decyl Sulfate Removal

Using the desalting tube "Solnac Tube" for LC/MS! Online removal of dodecyl sulfate.

When analyzing highly polar basic compounds using reversed-phase partition chromatography, adding acidic ionic species to the eluent can enhance retention by forming neutral ion pairs through ionic bonding. Sodium dodecyl sulfate, used as an ion-pairing reagent, is non-volatile and can precipitate in the ionization section of the MS, making it difficult to introduce, and it can suppress the ionization of the analytes, thus it cannot be used for online LC/MS measurements. In this case, we used a system with ammonium dodecyl sulfate (ADS) added, using caffeine and thiamine hydrochloride as samples, and removed dodecyl sulfate from the sample solution using a Solnack tube to perform positive ion measurements. For details on the conditions and analysis results, please download the catalog. 【Infusion Conditions】 ■Samples: (1) Caffeine 10 ppm solution, (2) Thiamine hydrochloride 10 ppm solution ■Solvent: CH3CN / H2O = 50 / 50 + 10 mM Ammonium dodecyl sulfate ■Flow rate: 0.1 ml/min *For more details, please refer to the PDF document or feel free to contact us.

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Application Data: Measurement of Positive Ions by Removal of Dibutylamine

Using the desalting tube "Solnac Tube" for LC/MS! DBA was removed online.

When analyzing highly polar acidic compounds using reversed-phase partition chromatography, adding basic ionic species to the eluent can enhance retention by forming neutral ion pairs through ionic bonding. In this case, nicotine acid and uracil acid were used as samples, and DBA in the sample solution was removed using a Sornak tube to conduct positive ion measurements. As a result, it was confirmed that Sornak is effective for LC/MS under mobile phase conditions containing ion pair reagents. For details on conditions and analysis results, please download the catalog. 【Infusion Conditions】 ■Sample: (1) Nicotinic acid 10 ppm solution, (2) Uracil acid 10 ppm solution ■Solvent: CH3CN / H2O = 50 / 50 + 0.1% DBA ■Flow rate: 0.1 ml/min *For more details, please refer to the PDF document or feel free to contact us.

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Application Data: Positive Ion Measurement by Triethylamine Removal

Using the desalt tube "Solnac Tube" for LC/MS! TEA was removed online.

When analyzing highly polar acidic compounds using reverse phase partition chromatography, adding basic ionic species to the eluent can enhance retention by forming neutral ion pairs through ionic bonding. Common basic mobile phases used for ion pair formation in LC/MS include triethylamine (TEA) and dibutylamine (DBA). However, when detecting positive ions, it is believed that ionization suppression occurs with almost 100% probability. In this case, nicotinic acid and uracil acid were used as samples, and TEA in the sample solution was removed using a solid-phase extraction tube for positive ion measurement. For details on conditions and analysis results, please download the catalog. 【Infusion Conditions】 ■Samples: (1) Nicotinic acid 10 ppm solution, (2) Uracil acid 10 ppm solution ■Solvent: CH3CN / H2O = 50 / 50 + 0.1% TEA ■Flow rate: 0.1 ml/min *For more details, please refer to the PDF document or feel free to contact us.

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[Application Data] Examples of improvements for easily adsorbed basic compounds

An example of improvement using post-column method for basic compounds that easily adsorb to the Sornak tube!

When using the Solnack tube CFAN under phosphate buffer conditions, if the compound being measured is basic, it may become dissociated and adsorb to the resin inside the tube. Therefore, by adding ammonia water using the post-column method before introducing the tube, we thought that making the eluent inside the tube basic and keeping the target compound in its non-dissociated form could suppress adsorption. We attempted to improve adsorption to the Solnack tube by adding ammonia water using the post-column method. For details on conditions and analysis results, please download the catalog. 【LC Conditions (Partial)】 ■ Equipment: Agilent 1200 ■ Detector: UV (215 nm) ■ Sample: 20 ppm solution of hydrochloride doxepin reagent ■ Injection volume: 5 μL ■ Post-column: 200 mM ammonia water at 0.05 ml/min *For more details, please refer to the PDF document or feel free to contact us.

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Application Data: Example of Negative Ion Measurement by TFA Removal (2)

Using the desalting tube "Sornak Tube" for LC/MS! The effect of TFA removal allows for signal detection.

When analyzing acidic compounds using reversed-phase partition chromatography, an acidic mobile phase (set to a pH that is at least 2 lower than the pKa of the analyte) may be used to suppress dissociation. Common acidic mobile phases suitable for use in LC/MS include acetic acid, formic acid, and trifluoroacetic acid (TFA). While TFA is appropriate for use at low pH, it is believed to cause ionization suppression with nearly 100% probability when detecting the analyte as a negative ion. Using methionine, an amino acid with acidic groups and high polarity, as the sample, TFA was removed from the eluent using a Sorbent tube, and negative ion measurements were conducted. For details on conditions and analysis results, please download the catalog. 【LC Conditions (Partial)】 ■ Equipment: Agilent 1200 ■ Flow rate: 0.3 ml/min ■ Detector: UV (210 nm) ■ Sample: Methionine 20 ppm solution ■ Injection volume: 5 μL *For more details, please refer to the PDF document or feel free to contact us.

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Application Data: Example of Negative Ion Measurement by TFA Removal

Using the desalting tube "Solnac Tube" for LC/MS! Removing TFA and conducting negative ion measurement.

When analyzing acidic compounds using reversed-phase partition chromatography, an acidic mobile phase (set to a pH more than 2 units lower than the pKa of the analyte) may be used to suppress dissociation. Common acidic mobile phases suitable for use in LC/MS include acetic acid, formic acid, and trifluoroacetic acid (TFA), with TFA being appropriate for use at low pH. However, TFA is considered to have too high an acidity, which can lead to ionization suppression with almost 100% probability when detecting the analyte as a negative ion. TFA was removed from the eluent using a Solnac tube, and negative ion measurements were conducted. For details on conditions and analysis results, please download the catalog. 【LC Conditions (Partial)】 ■ Equipment: Agilent 1200 ■ Flow rate: 0.3 ml/min ■ Detector: UV (210 nm) ■ Sample: Tryptophan 20 ppm solution ■ Injection volume: 5 μL *For more details, please refer to the PDF document or feel free to contact us.

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[Application Data] Example of Analysis of Cationic Surfactants

Application to ion pair reagents! Analysis example using the "Solnac Tube" for desalting in LC/MS.

Surfactants that change their properties at interfaces have both "hydrophilic" and "lipophilic" structural components within a single molecule. The hydrophilic part of surfactants often contains highly polar acids or bases, so in HPLC analysis, it is also possible to use a mobile phase with added ion-pair reagents such as sodium dodecyl sulfate (SDS). As a sample, a mixed solution of cationic surfactants such as tetrabutylammonium chloride and cetylpyridinium chloride was used for LC/MS measurements. For details on conditions and analysis results, please download the catalog. 【LC Conditions (Partial)】 ■ Equipment: Agilent 1200 ■ Flow rate: 0.3 ml/min ■ Detector: UV (215 nm) ■ Sample: Each 2.5 ppm solution ■ Injection volume: 5 μL *For more details, please refer to the PDF document or feel free to contact us.

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Application Data: Example of Ionic Liquid Analysis: Application to Ion Pair Reagents

Used the desalting tube "Solnac Tube" for LC/MS! Conducted online LC/MS analysis.

Ionic liquids are defined as "salts composed solely of ions that are in a liquid state at temperatures below 100°C," and their development is expected to focus primarily on their use as electrolytes. The main ionic liquids are often analyzed using HPLC with elution solutions that contain ion-pair reagents such as sodium dodecyl sulfate (SDS), which has high polarity and weak UV absorption, allowing detection even at low wavelengths. Using imidazolium salts, which are one of the representative structures of ionic liquids, we conducted LC/MS analysis with an elution solution containing ammonium dodecyl sulfate. For details on the conditions and analysis results, please download the catalog. 【LC Conditions (Partial)】 ■ Equipment: Agilent 1200 ■ Flow rate: 0.3 ml/min ■ Detector: UV (215 nm) ■ Sample: 5 ppm solution of 1-butyl-3-methylimidazolium chloride ■ Injection volume: 5 μL *For more details, please refer to the PDF document or feel free to contact us.

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Application data: Analysis of intact proteins

Using the desalting tube "Sornak Tube" for LC/MS! Reduces protein ionization suppression.

We will introduce the analysis of intact proteins using "Sornack Tube" by MS Solutions. In the analysis of intact proteins using reversed-phase partition chromatography, a mobile phase containing trifluoroacetic acid (TFA) is used. However, TFA has a high acidity, which is known to increase the current flowing between the needle and the counter electrode when used in LC-ESI/MS, thereby suppressing the ionization of the analytes. For details on conditions and analysis results, please download the catalog. 【LC Conditions (Partial)】 ■ Equipment: Agilent 1200 ■ Flow rate: 0.3 ml/min ■ Detector: UV (210 nm) ■ Sample: Protein each at 10 pmol/μL solution ■ Injection volume: 5 μL *For more details, please refer to the PDF document or feel free to contact us.

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Application Data: Attempts to Reduce Sodium Additive Ions

Using the desalting tube "Solnac Tube" for LC/MS! Removes trace amounts of sodium ions.

In positive ESI LC/MS analysis, it is known that sodium adduct ions ([M+Na]+) are easily observed, especially when methanol is used as the mobile phase. Depending on the analytical purpose, it may be necessary to reduce the intensity of [M+Na]+ and concentrate on protonated molecules ([M+H]+). We attempted to reduce the intensity of [M+Na]+ by removing trace amounts of sodium ions in the mobile phase using a sorbent tube. For details on the conditions and analysis results, please download the catalog. 【LC Conditions (Partial)】 ■ Equipment: Agilent 1200 ■ Flow rate: 0.3 ml/min ■ Detector: UV (230 nm) ■ Sample: 17α-methyltestosterone 50 ppm solution ■ Injection volume: 5 μL *For more details, please refer to the PDF document or feel free to contact us.

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Application Data: Example of Analysis of Narijikus Acid

Example of analyzing nalidixic acid using a desalting tube "Solnac Tube" for LC/MS!

We conducted an analysis using nalidixic acid, a type of quinolone antibacterial agent, as the sample under LC conditions with phosphate buffer solution. The confirmation test described in the pharmacopoeia employs ultraviolet-visible spectrophotometry, but since there was an example using phosphate buffer solution in Shiseido's application data, we referred to that. For details on the conditions and analysis results, please download the catalog. 【LC Conditions (Partial)】 ■ Equipment: Agilent 1200 ■ Flow rate: 0.3 ml/min ■ Detector: UV (215 nm) ■ Sample: Nalidixic acid reagent 20 ppm solution ■ Injection volume: 2 μL *For more details, please refer to the PDF document or feel free to contact us.

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Application Data: Example of Sulfonamide Analysis

Using the desalting tube "Solnac Tube" for LC/MS! We were able to measure four types of sulfonamides.

Sulfa drugs are a group of chemotherapeutic agents based on sulfanilamide, used as veterinary pharmaceuticals. An example using phosphate buffer solution was included in Shiseido's application data, so I referred to that to consider the elution conditions. For details on the conditions and analysis results, please download the catalog. 【LC Conditions (Partial)】 ■ Equipment: Agilent 1200 ■ Flow rate: 0.3 ml/min ■ Detector: UV (215 nm) ■ Sample: Mixed solution of 4 types of sulfa drugs at 20 ppm ■ Injection volume: 4 μL *For more details, please refer to the PDF materials or feel free to contact us.

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Application Data: Example of Erythromycin Impurity Analysis

Using the 'Solnac Tube' deionization tube for LC/MS! The official pharmacopoeia detects at 215nm.

Erythromycin, one of the macrolide antibiotics that has applications for many infectious diseases such as respiratory and soft tissue infections, was analyzed using LC conditions with phosphate buffer as the sample. Due to its weak UV absorption, erythromycin requires detection at a low wavelength, and it is detected at 215 nm in the pharmacopoeia. For details on the conditions and analysis results, please download the catalog. 【LC Conditions (Partial)】 ■ Equipment: Agilent 1200 ■ Flow rate: 0.3 ml/min ■ Detector: UV (215 nm) ■ Sample: Erythromycin reagent 50 ppm solution ■ Injection volume: 5μL *For more details, please refer to the PDF document or feel free to contact us.

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Development of an Online Desalting Tube Automatic Switching Device for LC/MS

Developed a device capable of continuous switching of 100 Solnac tubes! Includes applications such as "desalination tube examples."

This document introduces the development of an online desalting tube automatic switching device for LC/MS. It includes topics such as "LC/MS under non-volatile buffer conditions," "negative ion measurement results for methionine," and "system overview using the automatic switching device." The development of this device and system is being conducted with subsidies from the 2020 Hamamatsu City New Industry Creation Project and the 2021 Shizuoka Prefecture University-Founded Venture Business Acceleration and Promotion Project. We encourage you to read it. 【Contents (excerpt)】 ■ LC/MS under non-volatile buffer conditions ■ Example of phosphate buffer usage ■ Development of desalting tube ■ Application examples of desalting tube ■ Measurement examples of negative ions by TFA removal *For more details, please refer to the PDF document or feel free to contact us.

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Contracted services for liquid chromatography-mass spectrometry (LC/MS)

Demonstrates power in qualitative and quantitative analysis of trace components in complex mixed samples.

LC/MS is an analytical method that allows for the separation of components in a liquid mixture sample using LC, followed by the sequential acquisition of mass spectra. Compared to other analytical methods, it is characterized by high sensitivity and high selectivity, demonstrating its power in the qualitative and quantitative analysis of trace components in complex mixtures. It is used in various fields such as measuring drug concentrations in blood, analyzing drug metabolites, analyzing antibody drugs, researching disease-related markers, analyzing environmental pollutants, analyzing organic materials, and food analysis. We utilize two types of high-resolution LC-MS/MS and triple quadrupole LC-MS to provide various contract analyses related to LC/MS for both qualitative and quantitative purposes. In particular, for qualitative analysis using high-resolution LC-MS/MS, we undertake not only data measurement but also the structural estimation of unknown compounds. *For more details, please feel free to contact us.*

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Imaging mass spectrometry contract services

We provide data that assists in the analysis of the pharmacokinetics, toxicity prediction, and efficacy analysis of compounds!

We offer imaging mass spectrometry that allows us to obtain molecular information at various measurement points in biological samples, combined with spatial information, enabling the acquisition of comprehensive molecular maps. In addition to the matrix-assisted laser desorption/ionization method, we have developed a highly sensitive desorption electrospray ionization method. This high-sensitivity DESI can detect approximately 70-80% of the tested compounds. Customers can choose the imaging mass spectrometry method that best suits their needs from the two ionization techniques available. 【Lineup】 ■ Matrix-Assisted Laser Desorption/Ionization (MALDI) ■ Desorption Electrospray Ionization (DESI) *For more details, please feel free to contact us.

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