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首页> 外文期刊>Forensic science international >Ethyl glucuronide determination in meconium and hair by hydrophilic interaction liquid chromatography-tandem mass spectrometry.
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Ethyl glucuronide determination in meconium and hair by hydrophilic interaction liquid chromatography-tandem mass spectrometry.

机译:亲水作用液相色谱-串联质谱法测定胎粪和头发中的乙醛糖醛酸乙酯。

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摘要

Ethyl glucuronide (EtG) detection in non-conventional matrices, such as hair and meconium, can provide useful information on alcohol abuse over a long time frame, for example during pregnancy or after a withdrawal treatment. This study reports on the development, validation and application of a new hydrophilic interaction liquid chromatography-tandem mass spectrometry (HILIC-MS/MS) method for the analysis of EtG in meconium and hair. For each matrix, the sample preparation and the chromatographic separation were thoroughly optimised. Additionally, experiments with reversed-phase liquid chromatography were also performed in the development stages. Analyses were carried out using a Phenomenex Luna HILIC column (150 mm x 3 mm, 5 microm) and a mobile phase composed by ammonium acetate 2mM and acetonitrile, in gradient. Different SPE cartridges (Oasis MAX, Oasis WAX, aminopropyl silica) and solvents were tested in order to obtain the highest recoveries and cleanest extracts. Optimal results were obtained for meconium with aminopropyl cartridges, while for hair an incubation of 16 h with 2 mL of water and acetonitrile (50/50, v/v) provided good results. The analytical method was validated for both matrices (meconium and hair) by assessing linearity, precision, accuracy, recovery and limit of quantification. The calibration curve concentrations ranged from 50 to 1200 pg/mg for meconium and from 20 to 1000 pg/mg for hair. Real meconium and hair samples were analyzed and results were consistent with literature.
机译:非常规基质(例如头发和胎粪)中的乙醛糖醛酸乙酯(EtG)检测可以提供长时间的酒精滥用有用信息,例如在怀孕期间或戒断治疗后。这项研究报告了开发,验证和应用的一种新型的亲水相互作用液相色谱-串联质谱(HILIC-MS / MS)方法来分析胎粪和头发中的EtG。对于每种基质,样品制备和色谱分离都得到了彻底优化。另外,在开发阶段还进行了反相液相色谱实验。使用Phenomenex Luna HILIC色谱柱(150 mm x 3 mm,5微米)和由2mM醋酸铵和乙腈组成的流动相进行梯度分析。测试了不同的SPE柱(Oasis MAX,Oasis WAX,氨丙基硅胶)和溶剂,以得到最高的回收率和最干净的提取物。用氨丙基药筒获得最佳的胎粪效果,而将头发与2 mL水和乙腈(50/50,v / v)一起孵育16 h可得到最佳结果。通过评估线性,精密度,准确度,回收率和定量限,对两种基质(胎粪和毛发)均验证了该分析方法的有效性。胎粪的校准曲线浓度范围为50至1200 pg / mg,毛发的校准曲线浓度为20至1000 pg / mg。分析了真正的胎粪和头发样本,结果与文献一致。

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