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The worldwide consumption of illicit drugs presents a big problem in terms of health care and prosecution. In the recent years, hundreds of novel psychoactive substances came up and were traded via the Internet, but there is still a big demand for classic illicit drugs such as cocaine, heroin, cannabis and ecstasy. Among these, cocaine particularly is frequently altered not only with excipients, but also with other physiologically active substances. The purpose of this work was to estimate the trend of cocaine purity and abundance of its adulterants in samples seized by Austrian police from 2012 to 2017. A micro-HPLC method for quantification of cocaine and its most common adulterants was developed and validated using gradient elution and UV detection at four wavelengths. 110 cocaine samples were analysed. In all the samples cocaine was present as hydrochloric salt. Caffeine, procaine, levamisole, phenacetin, lidocaine and benzocaine were the most abundant adulterants.

Objectives: the development of a simple, rapid, sensitive, and accurate HPLC-UV method for the simultaneous determination of retinol and α-tocopherol in human plasma, suitable for the evaluation of these vitamins in pregnant women suffering from intrahepatic cholestasis of pregnancy (ICP). (b) Design and methods: chromatographic separation of vitamins was achieved with a microcolumn BDS HYPERSIL C18 (100 mm × 2.1 mm, 2.4 μm) using a C18 guard column. The developed and validated HPLC method proposed in this study was applied in the assessment of plasma concentrations of retinol and α-tocopherol in normal pregnancy (n = 37) and in pregnancy complicated with ICP (n = 19). (c) Results: the validation of the method showed excellent linearity for retinol and α-tocopherol (r2: 0.998 and 0.997), high sensitivity (LOD: 0.02 and 0.11 μM, LOQ: 0.07 and 0.36 μM), and high recovery (96.0–104.0% and 99.3–102.0%), respectively. The method requires a low sample volume and all procedures of sample preparation and analytical determination take less than 20 min to be completed. The evaluation of the results in ICP patients showed that α-tocopherol significantly diminished compared to normal pregnant women (13.1 ± 2.9 vs. 22.4 ± 2.2 μM, p < 0.05) whereas retinol remains unchanged (1.27 ± 0.21 vs. 1.25 ± 0.10 μM). (d) Conclusions: a simple, accurate, reliable, selective, highly sensitive and cost effective method suitable for routine determination of retinol and α-tocopherol in biological samples is proposed. It was possible to determine the decrease of α-tocopherol in ICP patients by this method. Fil: Martinefski, Manuela Romina. Universidad de Buenos Aires. Facultad de Farmacia y Bioquímica. Departamento de Química Analítica y Fisicoquímica; Argentina. Consejo Nacional de Investigaciones Científicas y Técnicas; Argentina Fil: Scioscia, Silvia. Universidad de Buenos Aires. Facultad de Farmacia y Bioquímica. Departamento de Tecnología Farmacéutica; Argentina Fil: Contin, Mario Daniel. Universidad de Buenos Aires. Facultad de Farmacia y Bioquímica. Departamento de Química Analítica y Fisicoquímica; Argentina. Consejo Nacional de Investigaciones Científicas y Técnicas; Argentina Fil: Samassa, Paula. Universidad de Buenos Aires. Facultad de Farmacia y Bioquímica. Departamento de Química Analítica y Fisicoquímica; Argentina Fil: Lucangioli, Silvia Edith. Universidad de Buenos Aires. Facultad de Farmacia y Bioquímica. Departamento de Tecnología Farmacéutica; Argentina. Consejo Nacional de Investigaciones Científicas y Técnicas; Argentina Fil: Tripodi, Valeria Paula. Universidad de Buenos Aires. Facultad de Farmacia y Bioquímica. Departamento de Tecnología Farmacéutica; Argentina. Consejo Nacional de Investigaciones Científicas y Técnicas; Argentina

医薬部外品の薬事申請用試験及び安定性を中心とした品質管理試験等には, 効率化のためグラディエントHPLC法による多薬剤同時分析法が多く用いられている。本報では, 溶媒使用量が汎用HPLCの1/10程度に削減可能なセミミクロHPLC装置を用い, 汎用HPLCで設定した分析条件の直接適用可能性及び分析精度等の基本的検討を行った。また, 実試料例として6薬剤配合の育毛剤を用い, 複雑なグラディエント法による定量分析への応用を検討した。保持時間の再現性は良好であり, 注入量の再現性に関しても2μl以上ではC.V.%1-2%程度であり, 良好であった。また, グラディエント法では, 高濃度有機溶媒領域で保持時間が若干早くなる現象が見られたが分離に影響はなく, 微量金属の影響を受けやすいヒノキチオールのピークに関しても良好であった。6薬剤配合育毛剤の定量分析において汎用HPLCの精度と同様な値であることが確認された。

Micro-HPLC separation and UV detection of some metal thenoyltrifluoroacetonates has been achieved. Cyano, octadecyl, and HTT A modified silica gels were used as stationary phases. Data about separation and detection parameters optimization are also described.

The generation of a micro-gradient for micro HPLC capillary columns is described. The system used is a modified and improved version of a split flow gradient elution device. Gradient tests have been performed and have shown good reproducibility under all conditions. The system has been successfully coupled with a particle beam LC-MS interface and the analysis of a mixture of twenty seven basic or neutral pesticides is reported.

Thermal lensing (TL) permits ultrasensitive measurements of optical absorption of analytes in very small volumes. Separation-detection conditions of non-labeled amino acids with micro-HPLC/UV absorption detector are optimized, and direct determination of non-labeled amino acids by micro-HPLC/UV-excitation TL detection in a gradient elution is successfully demonstrated. Non-labeled amol-level amino acids is detectable with the TL detection system, which has thousand times better sensitivity than a conventional UV detector.

Plastic tubing of polyetheretherketone (PEEK) is used for the preparation of HPLC packed capillary columns. The polymer is rigid but not fragile, has great resistance to chemical and physical agents and comes in standard 1/16″ O.D. These features can extend the column lifetime and facilitate the overall employment of HPLC capillary columns. Serial connection of short columns is also possible with no increase in dead volume. A new, rapid and effective packing method has been developed to be compatible with the characteristics of the material. Several C8 and C18 columns have been prepared and tested and some applications are shown.

A new method is introduced for packing micro-columns with an ID (inner diameter) of 320 μm. The advantage of this method is the extraordinary economy of the packing material employed and the high reliability in production. The theoretical plate height ranges from 7 to 8 μm for 3 μm particles.

低級脂肪族アミン及び置換フェノール類を塩化4-ジメチルアミノアゾベンゼン-4'-スルホニル(Dabsyl-Cl)と反応させ,又脂肪族アルデヒドはダブシルヒドラジンと反応させダブシルヒドラゾンとして共鳴ラマン効果が期待できる誘導体に変換した.これらの誘導体は逆相セミミクロカラム(μS-Finepak C18,1.5mmφ×250mm)で分離後,その溶離成分をアルゴンイオンレーザー488.0nmの発振波長を用いて1136cm-1で共鳴ラマン検出を行った.レーザー出力,スリット幅,スムージング数など検出感度に影響を与える要因の検討を行い,ラマン検出の最適条件を調べた.その結果,従来の内径4,6mmのカラムを使用したLC/ラマン検出と比べて検出限界は絶対注入量で20倍向上し,2ngまで検出可能であった.

長鎖脂肪族カルボン酸の誘導体化試薬として,Arイオンレーザーの励起光に近接した波長領域に吸収を示す4-ニトロ-4'-N・メチル,N・β-ヒドロキシエチルアミノアゾベンゼンを合成した.カルボン酸は二塩化オキサリルで酸クロライドとした後,誘導体化試薬を用いてエステル誘導体とした.これらの誘導体は逆相セミ・ミクロカラムで分離後,その溶離成分を1343cm-1のラマンバンドに設定して共鳴ラマン検出した.その結果,ラウリン酸では5～200ppmの濃度範囲で検量線は直線を示した.20 ppmでの相対標準偏差(n=5)は4.4%と良好であった.

The interface for direct coupling of micro HPLC with FAB mass spectrometry has been evaluated as a simple sample introduction system using unstable and/or non-volatile compounds having higher molecular weight. The good reproducibility of chromatograms, little fluctuation and small tailing in chromatographic peak profiles, and the excellent quality of mass spectral patterns were obtained. High-molecular-weight compounds such as parathyroid hormone and insulin chain B could be introduced and ionized stably with high sensitivity.

The separation of polycyclic aromatic hydrocarbons (PAH) on various reversed-phase columns (phenyl, ethyl, octyl and octadecyl) have been compared. The correlations between the logarithm of capacity factor (log k′) and several descriptors, which show the molecular size, shape and physical property of a solute, were determined. The results indicated the high possibility to predict the retention of PAH in reversed-phase high performance liquid chromatography.