臨床、法医、中毒学

Articles

4.5 Minute Analysis of Benzodiazepines in Urine and Whole Blood Using LC/MS/MS and an Ultra Biphenyl Column

Sample throughput for benzodiazepines in urine and whole blood can be increased by adopting this dilute-and-shoot LC/MS/MS method which uses an Ultra Biphenyl HPLC column. Partial validation data are presented in this application note.

Featured Application: Creatine and Creatinine in Plasma and Urine on Raptor HILIC-Si

A rapid, robust method was established for the analysis of creatine and creatinine in human plasma and urine. An efficient separation was achieved in less than 1.5 min using a Raptor HILIC-Si column and a simple isocratic mobile phase.

Featured Application: Derivatized Amphetamines on Rxi-5Sil MS

GC analysis of derivatized amphetamines and other drugs of abuse can be improved by using Rxi-5Sil MS columns. Robust and highly inert, these columns withstand harsh conditions, such as exposure to the derivatization reagents. High inertness and enhanced stability result in good peak shape and response, low phase bleed, and longer column lifetimes.

Featured Application: Raptor HILIC-Siを用いた血しょう中葉酸欠乏症バイオマーカー分析

LC-MS/MSによる血しょう中の葉酸欠乏症バイオマーカー分析は、マトリックスとなるリン脂質およびリゾリン脂質により複雑化されます。これらはサプレッションの原因となり、分析精度を悪くし、MSイオンソースの汚染原因ともなるため逆相モードにおいて問題となります。ここで紹介するRaptor HILIC-SiカラムによるHILICモードでの分析では、葉酸欠乏症バイオマーカーとマトリックスとを完全に分離し、短時間で精確な測定をおこなうことができます。

Featured Application:Foce C18を用いた全血中の γ-ヒドロキシ酪酸 (GHB) の分析

γ-ヒドロキシ酪酸(GHB)およびその前駆体であるγ-ブチ路ラクトンと1,4-ブタンジオールのLC-MS/MSによる直接分析法は、分析時間5分での同時分析が可能です。内因性の低濃度GHB測定や外因性の薬物使用を測定するのに十分な感度も得られました。

Featured Application: Force C18を用いたメチルマロン酸(MMA)分析

メチルマロン酸分析は、ビタミンB12欠乏症およびメチルマロン酸血症を診断するのに重要な臨床検査です。通常、煩雑な前処理を必要とし、かなりの時間とコストがかかります。ここで開発したLC-MS/MS法は、タンパク質変性サンプルの上清をForce C18カラムに直接導入するだけで、アイソバリック化合物からのクロマトグラフィー分離も可能なより簡便な方法です。

Featured Application: Raptor FluoroPhenyl を使用した血液中ホスファチジルエタノールの分析

ホスファチジルエタノール(PEth)の正確な分析を、簡単なタンパク質沈殿法と3.5分のグラジエント分析によるLC-MS / MS法でおこなうことができます。ここでは、Raptor FluoroPhenylカラムを使用したメソッドを紹介しており、飲酒によるアルコールのバイオマーカーとしてPEthをモニタリングするラボに低コストかつハイスループットなソリューションを提供します。

Featured Application: Urinary Free Cortisol and Cortisone on Raptor Biphenyl

In general, LC-MS/MS analysis of urinary free cortisol and cortisone can provide better specificity than immunoassay-based methods. However, it is critical that the analytical column has the proper selectivity for chromatographically separating cortisol from isobaric matrix components. In the method presented here, complete separation of the target analytes and matrix interferences was obtained in a 3-minute analysis on a Raptor Biphenyl column.

A Fast Dilute-And-Shoot Method for Simultaneous 5-Hydroxyindoleacetic Acid (5-HIAA), Vanillylmandelic Acid (VMA), and Homovanillic Acid (HVA) LC-MS/MS Analysis in Human Urine

Using Restek’s dilute-and-shoot method and a Raptor Biphenyl column, serotonin and catecholamine metabolites can be measured simultaneously in a quick 5-minute analysis. This method is applicable to clinical 5-HIAA, VMA, and HVA LC analysis in urine and provides the benefit of both fast analysis times and low-cost sample preparation procedures.

A Novel Solution for Vitamin K1 and K2 Analysis in Human Plasma by LC-MS/MS

Vitamin K1 and K2 analysis is typically complex and time-consuming because these lipophilic vitamins occur at low levels and are subject to matrix interference, particularly from phospholipids. The new method established here provides fast, accurate, and precise vitamin K levels in plasma using a simple phospholipid removal procedure and a sensitive 4-minute LC-MS/MS analysis on a Raptor Biphenyl column, making it suitable for high-throughput testing.

Analysis of Fentanyl and Its Analogues in Human Urine
by LC-MS/MS

Synthetic opioid drugs, such as fentanyl and sufentanil, have very high analgesic potency. Abuse of these prescription painkillers—along with a rapidly growing list of illicit analogues—is a significant public health problem. In this study, we developed a simple dilute-and-shoot method that provides a fast 3.5 minute analysis of fentanyl and related compounds (norfentanyl, acetyl fentanyl, alfentanil, butyryl fentanyl, carfentanil, remifentanil, and sufentanil) in human urine by LC-MS/MS using a Raptor Biphenyl column.

Analysis of Synthetic Cannabinoids and Metabolites: Adding New Compounds to an Existing LC-MS/MS Method

The analysis of synthetic cannabinoids and their metabolites can be a difficult and challenging task. Keeping up with the ever-growing list of synthetic cannabinoids that illicit drugmakers produce further complicates the analysis. As shown here, the retention and selectivity of the Raptor Biphenyl column allows new drugs to be added to an existing method, providing labs with an important vehicle for improving efficiency and productivity.

Definitive EtG/EtS LC-MS/MS Analysis: A Rugged 4-Min Method for High-Throughput Labs

By properly conditioning new columns and employing Restek’s EtG/EtS method for sample prep and analysis, high-throughput labs testing human urine samples for these alcohol consumption biomarkers can ensure accurate, consistent results with fewer column changes.

Direct Analysis of Morphine, M3G and M6G Metabolites, and Related Compounds in Urine by LC-MS/MS

The analysis of total morphine is typically conducted by first subjecting urine samples to acid or enzymatic hydrolysis in order to cleave the glucuronide conjugates off of morphine’s primary metabolites [morphine-3β-D-glucuronide (M3G) and morphine-6β-D-glucuronide (M6G)] prior to analysis. With the glucuronide moiety removed, the resulting morphine molecule is much less polar and, therefore, more amenable to traditional reversed-phase chromatography than the metabolites are. However, both hydrolysis procedures cost an analyst time and result in sample variability due to incomplete hydrolysis or analyte conversion. By utilizing the retention characteristics of the Restek Force Biphenyl column, hydrolysis was not required and direct analysis of morphine, its M3G and M6G metabolites, and several related compounds using a simple “dilute-and-shoot” sample preparation was performed.
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Dissecting Raptor LC Columns: A closer look at a new species

When we engineered our superficially porous particle (SPP or "core-shell") Raptor LC columns, we developed the bonding chemistries that are best suited to both the SPP construction and our highly selective USLC phases. But we didn't stop here. Take a closer look at a new species as we dissect the upgraded hardware and new, proprietary packing techniques behind Raptor LC columns and Raptor EXP guard columns. (PDF - 1725kB)

Fast Screening and Confirmation of Gamma-Hydroxybutyrate (GHB) in Urine

The headspace (HS) analysis of gamma-hydroxybutyrate (GHB) described here reduces contamination and eliminates time-consuming derivatization. Confirmation testing using an Rtx-5MS column, provides definitive results in less than 7 minutes.

Fast Screening of Recalled Tylenol for Tribromoanisole and Related Adulterants Using QuEChERS and GC-TOFMS

Screening methods for consumer product adulteration cases, such as the recent Tylenol recall, can benefit from fast QuEChERS-based sample preparation and sensitive, full mass-range GC/TOF-MS.
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Fast, Definitive Data for Blood Alcohol Testing on Rtx-BAC Plus 1 and Rtx-BAC Plus 2 Columns

Rtx-BAC Plus 1 and Rtx-BAC Plus 2 columns provide definitive data in a fast, 2-minute analysis, so you can be certain of your results, maximize sample throughput, and get accurate, reliable results quickly, which is is critical for analyzing blood alcohol concentration (BAC). (PDF - 963kB)

GC Inlet Liner Deactivations for Basic Drug Analysis

Basic drugs can interact with active sites on the surface of the inlet liner, reducing responses. The combination of a base-deactivated liner and a base-deactivated Rtx-5Amine column ensures the greatest responses in analyses for these compounds.

LC-MS/MSを用いた全血中免疫抑制剤のハイスループット分析

臓器移植の成功は、免疫抑制剤の正確かつタイムリーな分析に大きく依存します。本検討では、全血中のシクロスポリンA、タクロリムス、シロリムスおよびエベロリムスの迅速かつ正確な方法を開発しました。ここでは、Raptor Biphenylカラムを用いたLC-MS/MS分析とタンパク質沈殿による前処理のみを組合わせ、マトリックスの影響を受けずに、3分という高速分析をおこなうことができました。直線性、堅牢性、精確さおよび精度において優れた結果が得られ、この方法が治療薬物モニタリングにおけるハイスループット分析に適していることが示されました。

Overcoming the Effects of Highly Organic Protein Precipitation Extracts on LC Peak Shape Using Direct Injection

Protein precipitation is frequently used to minimize matrix impact when analyzing biological samples. However, the effects of highly organic protein precipitation sample extracts on LC peak shape can negatively impact accurate quantification. Dilution or further sample preparation steps are often used to minimize these effects; however, here we show that direct injection of sample extracts is a viable option that can be used to prevent peak distortion, while avoiding the time and variability associated with additional sample preparation.

Rapid Analysis of 17 Bile Acids in Human Plasma
by LC-MS/MS

Quantitative analysis of bile acids in plasma is critical for diagnosing liver disease as well as assessing drug safety. Accurate reporting can be difficult because of analyte characteristics, matrix effects, and other factors. Here, we establish a rapid, robust, and selective LC-MS/MS method for the analysis of bile acids in human plasma using a Restek Raptor C18 column. One of the significant improvements over other reported methods was the baseline separation of all 17 bile acids in 6 minutes including three isomer groups.

Rapid Analysis of C3 Epimers of 25-Hydroxyvitamin D in Serum by LC-MS/MS

The C3 epimers of 25-hydroxyvitamin D have lower bioactivity than the primary metabolites and, unless they are chromatographically separated, can cause clinical vitamin D levels to be overestimated. Raptor FluoroPhenyl columns provide baseline resolution of all key compounds, and the method established here allows accurate quantification in a fast, 5-minute analysis time (7-minute total cycle time). This method is recommended for labs interested in reporting C3 epimer concentrations separately in order to obtain more accurate results for the clinical diagnosis of vitamin D status.

Rapid Analysis of Steroid Hormones by GC/MS

GC/MS analysis of urinary steroid hormones is a demanding application, and the Rxi-1ms column meets the requirements for low bleed and inertness better than any column we have tested. We analyzed a variety of derivatized steroid sex hormones in less than 25 minutes, with excellent resolution and symmetric peaks. At 300°C or above, bleed from the Rxi-1ms column was negligible.

Rapid and Accurate LC-MS/MS Analysis of Nicotine and Related Compounds in Urine Using Raptor Biphenyl LC Columns and MS-Friendly Mobile Phases

A rapid, accurate, and reproducible method was developed for high-throughput testing of nicotine, cotinine, trans-3'-hydroxycotinine, nornicotine, norcotinine, and anabasine in urine. Data show that a fast and highly efficient analysis of these basic compounds can be achieved with the Raptor Biphenyl column using standard, low pH, reversed-phase LC-MS mobile phases which are compatible with a variety of LC-MS instrumentation.
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Raptor Biphenyl LC Columns Brochure

Raptor LC columns combine the speed of superficially porous particles (i.e., SPP or “core-shell”) with the resolution of highly selective USLC technology. Featuring Restek's most popular LC stationary phase, the rugged Raptor Biphenyl is extremely useful for fast separations in bioanalytical testing applications like drug and metabolite analyses, especially those that require a mass spectrometer (MS). (PDF - 6071kB)

Reduce Downtime and Cost of Materials with Rugged Rxi-5Sil MS GC Columns

New Rxi-5Sil MS columns produce consistent results for amphetamine—even after 400 injections of derivatizing reagent—resulting in less time and money spent on column maintenance and replacement.

Reliably Confirm Cannabinoids by GC-MS

Screening for evidence of marijuana use is typically done using an immunoassay method to detect derivatives in urine, but confirmation of positive results requires GC-MS. Here we describe a GC-MS method, using an Rxi-5ms column, that resolves all major cannabinoid metabolites to baseline and exhibits very low bleed, even at 300 °C. We also prolonged column life by baking at 340 °C to remove derivatization by-products.
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Rtx-BAC Plus 1 and Rtx-BAC Plus 2 Columns

Rtx-BAC Plus 1 and Rtx-BAC Plus 2 columns provide definitive data in a fast, 2-minute analysis, so you can be certain of your results, maximize sample throughput, and get accurate, reliable results quickly, which is is critical for labs analyzing blood alcohol concentration (BAC). (PDF - 5471kB)
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Rxi-5Sil MS Columns: Assured Performance for Forensic Applications

Rxi-5Sil MS columns produce excellent results for a number of forensic applications. The versatile selectivity separates a wide variety of compounds, which lets you keep analyzing samples instead of changing columns between methods. (PDF - 0kB)

Sensitive GC/MS Analysis for Drugs of Abuse

An Rxi-5ms column will resolve acidic/neutral or free basic drugs under one set of conditions. There is no interference from column bleed — not even at 330°C. This is one of the first published applications for our new family of Rxi columns.

Simultaneous Analysis of Catecholamines and Metanephrines in Urine by LC-MS/MS

Clinical diagnosis of pheochromocytoma and paraganglioma is often based on the analysis of catecholamines (epinephrine, norepinephrine, dopamine) and metanephrines (metanephrine, normetanephrine, 3-methoxytyramine) in urine. Analysis of these polar compounds using reversed-phase LC can be difficult due to limited chromatographic retention, which results in poor separation of the analytes from closely eluting matrix interferences. This method overcomes these problems by combining a simple solid phase extraction procedure with the consistent and accurate chromatographic performance of a Raptor Biphenyl column.

Tech Tip: Column Conditioning Ensures Consistent EtG/EtS Results

Methods for monitoring alcohol consumption biomarkers EtG and EtS are generally limited by poor retention and coelution with matrix interferences, as well as by long analysis times and short column lifetimes. The dilute-and-shoot EtG/EtS LC-MS/MS analysis developed here using the novel Raptor EtG/EtS column easily resolves EtG and EtS from matrix interferences, providing consistent, accurate results for high-throughput labs testing human urine samples for alcohol consumption.
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Thermal Desorption: A Practical Applications Guide: III. Defence and Forensic

Thermal desorption is used extensively for forensic science. This 16-page publication from Markes International Ltd. presents several key applications including drugs, arson accelerants, trace explosives, shotgun propellant, and inks. (PDF - 0kB)

Trace-Level Analysis of Metanephrines in Plasma by HILIC LC-MS/MS

Highly sensitive analysis of metanephrines and in plasma is critical in the diagnosis and treatment of pheochromocytoma and paraganglioma. Here, a HILIC LC-MS/MS method was developed using a Raptor HILIC-Si column because this approach provides retention of all target compounds in highly organic mobile phases, thus providing the increased sensitivity needed to reach low detection limits. Data from linearity, accuracy, and precision testing demonstrate that accurate results are consistently obtained—even at trace levels—for these important clinical biomarkers.

USLC Columns Put the Right Tools in Your LC Method Development Toolbox

Column selectivity has the most significant influence on chromatographic peak separation, or resolution, so choosing the right column can greatly speed up HPLC and UHPLC method development. In this article, we discuss column choice and identify a set of just 4 stationary phases—Restek’s USLC column set—that encompasses the widest range of reversed phase selectivity available today.
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Versatile GHB Method For Headspace or Liquid Injection

The headspace (HS) analysis of gamma-hydroxybutyrate (GHB) described here reduces contamination and eliminates time-consuming derivatization. Confirmation testing using an Rtx-5MS column, provides definitive results in less than 7 minutes. (PDF - 0kB)

LC-MS/MSによる231種類の薬物およびその代謝物のための分析法の開発

薬物分析の需要が増加するにつれ、多くのラボが時間短縮や感度、特異性を向上させるためにLC-MS/MS法に取り組みつつあります。ここに示す方法では、Raptor Biphenylカラムを使用しているため、231種類の薬物およびその代謝物の迅速かつ正確な分析が可能となりました。