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首页> 外文期刊>Forensic science international >A rapid screening procedure for drugs and poisons in gastric contents by direct injection-HPLC analysis.
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A rapid screening procedure for drugs and poisons in gastric contents by direct injection-HPLC analysis.

机译:通过直接进样-HPLC分析快速筛查胃内容物中的药物和毒物。

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A high performance liquid chromatographic method for toxicological drug screening of gastric content has been developed. The samples were diluted (1:3-1:30) in 0.01N hydrochloric acid and injected into a reverse phase column for separation by gradient elution. Mobile phase consisted of solvent A (acetonitrile/water 90:10, 0.01M sodium dodecylsulphate, 0.5% v/v glacial acetic acid) and solvent B (water/acetonitrile 90:10, 0.01M sodium dodecylsulphate, 0.5% v/v glacial acetic acid); the gradient was programmed from 20 to 80% A in 30min. The flow was kept constant at 1.5ml/min. Two home-made internal standards, butyrylsalicylic acid and diacetyltubocurarine with retention times of 5.6 and 21.4min, respectively, were used. Drugs are identified by matching their relative retention times and UV spectra (200-400nm) with those contained in a home made library of more than 340 reference compounds (9 analgesics, 22 antidepressants, 30 antihistamines, 14 antihypertensives, 21 antirheumatics, 15 beta-blockers, 9 bronchodilators, 10 Ca antagonists, 14 diuretics, 26 neuroleptics, 25 tranquilizers, and other significant xenobiotic compounds). The fluorometric (FLD) emission spectrum (280-700nm; excitation wavelength, 230nm) was used as a further identification. At 50mg/l analyte concentrations, the injection of gastric content after dilution (1:3) produced S/N ratios in the range 8-140. The method is simple, rapid, rather inexpensive and proved to be a useful means of investigation if used in combination with GC-MS screening in blood. On the other hand, the system suffers from a relatively limited sensitivity for compounds with a low UV absorption and from interferences due to the presence in the matrix of some highly UV- and FL-responsive compounds (e.g. tryptophan).
机译:已经开发出一种用于胃内容物毒理学药物筛选的高效液相色谱方法。将样品在0.01N盐酸中稀释(1:3-1:30),然后注入反相柱中,通过梯度洗脱进行分离。流动相包括溶剂A(乙腈/水90:10、0.01M十二烷基硫酸钠,0.5%v / v冰醋酸)和溶剂B(水/乙腈90:10、0.01M十二烷基硫酸钠,0.5%v / v冰醋酸)醋酸);在30分钟内将梯度从20%A设置为80%A。流量保持恒定在1.5ml / min。使用了两种自制的内标物,丁酰水杨酸和二乙酰基微管尿素,保留时间分别为5.6和21.4min。通过将其相对保留时间和UV光谱(200-400nm)与包含340多种参考化合物的自制库(9种镇痛药,22种抗抑郁药,30种抗组胺药,14种抗高血压药,21种抗风湿药,15种β-阻滞剂,9种支气管扩张药,10种钙拮抗剂,14种利尿药,26种抗精神病药,25种镇静剂和其他重要的异种生物化合物)。荧光(FLD)发射光谱(280-700nm;激发波长,230nm)被用作进一步的鉴定。在50mg / l的分析物浓度下,稀释(1:3)后注入胃液产生的信噪比范围为8-140。该方法简单,快速,相当便宜,并且如果与血液中GC-MS筛查结合使用,将被证明是一种有用的研究方法。另一方面,该系统对具有低UV吸收的化合物具有相对有限的敏感性,并且由于一些对UV和FL具有高响应性的化合物(例如色氨酸)在基质中的存在而受到干扰。

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