Determination of zolpidem in human hair by micropulverized extraction based on the evaluation of relative extraction efficiency of seven psychoactive drugs from an incurred human hair specimen
Determination of zolpidem in human hair by micropulverized extraction based on the evaluation of relative extraction efficiency of seven psychoactive drugs from an incurred human hair specimen
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基于人发标本中7种精神活性药物相对提取效率评价的微粉碎提取法测定人发中唑吡坦
DOI：
10.1016/j.chroma.2013.04.007
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发表时间：
2013
期刊：
影响因子：
4.1
通讯作者：
H
中科院分区：
文献类型：
--
作者：
Miyaguchi;H
建立了一种从毛发中快速提取精神药物的微粉碎方法。将头发样品（IOmg）用0.2mL的45%（w/v）磷酸铵水溶液（pH 8.4）在42 Hz下微粉碎10分钟。在同一管中使用乙腈进行液-液萃取，除去有机层并过滤。传统的方法，包括固液萃取与磷酸铵溶液或甲醇，也被采用，阿米替林，去甲替林，去甲氟地西泮，氟硝西泮，7-氨基氟硝西泮，米安色林和唑吡坦与这些方法从一个真实的人发标本的相对提取效率进行了比较，使用液相色谱/串联质谱。所有分析物的最高提取效率，实现使用这里开发的方法，即使提取时间（10分钟）很短。过夜甲醇提取经常用于毛发分析;然而，提取效率不足以用于胺。该方法已成功应用于人发中唑吡坦的定量分析。方法的定量范围为1- 25000 pg/mg，日间精密度和准确度（n=5）分别为1.8-8.8%和3.3- 8.1%。将开发的方法应用于3份实际（真实）样品，其中唑吡坦的浓度测定为78.9- 18，300（pg/mg）。
A micropulverization method for rapid extraction of psychoactive drugs from hair was developed. A hair sample (10mg) was micropulverized for 10min at 42Hz with 0.2mL of 45% (w/v) aqueous ammonium phosphate (pH 8.4). Liquid–liquid extraction was carried out in the same tube using acetonitrile, and the organic layer was removed and filtered. Conventional methods, including solid–liquid extraction with an ammonium phosphate solution or methanol, were also employed, and the relative extraction efficiencies of amitriptyline, nortriptyline, norfludiazepam, flunitrazepam, 7-aminoflunitrazepam, mianserin and zolpidem with these methods from an incurred human hair specimen were compared using liquid chromatography/tandem mass spectrometry. The highest extraction efficiencies for all the analytes were achieved using the method developed here, even though the extraction time (10min) was short. Overnight methanol extraction has frequently been used for hair analysis; however, the extraction efficiency was not sufficient for amines. The method was successfully applied to the quantification of zolpidem in human hair. The range of quantification was 1–25,000pg/mg, and interday accuracy and precision (n=5) at three concentrations were 1.8–8.8% and 3.3–8.1%, respectively. The developed method was applied to three actual (incurred) samples, for which the concentrations of zolpidem were determined to be 78.9–18,300 (pg/mg).