臨床、法医、中毒学

Articles

Featured Application: Raptor HILIC-Si による血しょうおよび尿中のクレアチン・クレアチニン分析

ヒト血しょうおよび尿中のクレアチンとクレアチニン分析の迅速かつ頑健な条件を検討しまし、Raptor HILIC-Siカラムとシンプルなイソクラティック移動相を使用した、1.5分以内の効率的な分離を達成できました。

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-ブチロラクトンと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: Raptor Biphenylによるメンタルヘルス薬

ヒト尿中58種の抗精神病薬と抗うつ薬の同時測定は、簡単なサンプル前処理手順と、Raptor Biphenyl カラムによる高速な5.5分のLC-MS / MS分析で実現します。 このメソッドは、正確でハイスループットな測定を提供し、臨床および法医学のモニタリングの両方に適しています。

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: Raptor Biphenylでの尿中遊離コルチゾールならびにコルチゾン分離

一般に、LC-MS/MSによる尿中の遊離コルチゾールおよびコルチゾン分析は、イムノアッセイに基づく方法よりも優れた特異性をもたらします。しかし、コルチゾールをアイソバリック化合物から分離する選択性がカラムには求められます。ここで紹介する方法では、Raptor Biphenylカラムを用いて3分という短時間でターゲット化合物とマトリックスによる干渉を完全に分離することが可能です。

高速Dilute-And-Shoot法による ヒト尿中の5-ヒドロキシインドール酢酸 (5-HIAA), バニリルマンデル酸(VMA)とホモ バニリン酸(HVA)の同時LC-MS/MS分析

Restekの dilute-and-shoot 法とRaptor Biphenylカラムを使用すると、セロトニンとカテコールアミンの代謝物を5分間で同時分析が可能です。このメソッドは5-HIAA、VMA、HVAのLC-MS/MS分析において、高速分析と低コストなサンプル前処理手順との組み合わせが要求される臨床検査のラボに適用できます。

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 Amphetamines by LC-MS/MS for High-Throughput Urine Drug Testing Labs

Accurate analysis of amphetamines by LC-MS/MS can be achieved using chiral columns, but the analysis presented here provides a simpler, more cost-effective approach for high-throughput labs. Excellent separation of all enantiomers in urine was obtained in a fast, 7-min quantitative analysis on a Raptor C18 column with no interference from matrix components.

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.

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.
PDF Document

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)

Evaluation of a Simple Method for Methylmalonic Acid Analysis in Human Plasma by LC-MS/MS

A new LC-MS/MS method for methylmalonic acid (MMA) analysis was developed that provides complete chromatographic resolution from isobaric succinic acid in plasma samples. Excellent chromatographic results were obtained from the direct injection of a protein crash sample supernatant onto a Force C18 column, providing a much simpler sample preparation compared to typical methods.

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.
PDF Document

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)

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。

Improved Screening Method for Acylcarnitines and Amino Acids in Dried Blood Spots by LC-MS/MS

This method for acylcarnitines and amino acids using LC-MS/MS with a guard cartridge column provides the speed of flow injection methods with improved sensitivity and specificity.

Method Evaluation: Analysis of Phosphatidylethanol (PEth) in Human Whole Blood by LC-MS/MS

The method established in this validation study provides accurate analysis of phosphatidylethanol (PEth) using a simple protein precipitation procedure and a fast 3.5 minute LC-MS/MS gradient run. Specific, sensitive analysis of PEth 16:0/18:1 in whole blood was obtained due to the unique selectivity and retention of the Raptor FluoroPhenyl column.

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.

1度のシンプルなSPE処理によるマトリックス由来のシグナルサプレッションを防止するリン脂質とタンパク質の除去

生体サンプルには、タンパク質とリン脂質が含まれています。これらはLC-MS/MS分析の妨害となり、装置のメンテナンス頻度を増やす可能性があります。ここでは、Resprep PLR SPEを使用し、1つの効率的なサンプル前処理を用い、血しょうからタンパク質とリン脂質を同時に除去しました。リン脂質の同時除去により、リン脂質によるシグナルサプレッションを受けずに幅広い化合物で優れた回収率が得られました。追加のメソッド開発も不要となります。

LC-MS/MSによるヒト血漿中胆汁酸17種類の高速分析

血漿中の胆汁酸の定量分析は,肝疾患の診断および薬剤の安全性評価において重要です。分析対象物の特性,マトリックス効果,およびその他の要因により,正確な結果を得ることは困難な場合があります。ここでは, Raptor C18カラムを使用して,迅速かつ堅牢で選択的なLC-MS/MS法による,ヒト血漿中の胆汁酸分析の分析法を開発しました。他に報告されている方法と比較して重要な改善点の1つは,3組の異性体を含む17種類すべての胆汁酸を6分間でベースライン分離できたことです。

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.
PDF Document

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.
PDF Document

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)
PDF Document

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)

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.

Successful Strategies for the Analysis of EtG and EtS in Urine

LC-MS/MS analysis of EtG and EtS is challenging due primarily to poor retention and resolution of EtG and EtS from matrix components. This article presents a foundation method that is useful for many samples and also demonstrates effective strategies for improving sensitivity and mitigating matrix effects.

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.
PDF Document

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.
PDF Document

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。

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