Development and validation of a rapid turboflow LC-MS/MS method for the quantification of LSD and 2-oxo-3-hydroxy LSD in serum and urine samples of emergency toxicological cases
Development and validation of a rapid turboflow LC-MS/MS method for the quantification of LSD and 2-oxo-3-hydroxy LSD in serum and urine samples of emergency toxicological cases
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DOI：
10.1007/s00216-014-8388-1
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发表时间：
2015-02-01
影响因子：
4.3
通讯作者：
Rentsch, Katharina M.
中科院分区：
文献类型：
--
作者：
Dolder, Patrick C.;Liechti, Matthias E.;Rentsch, Katharina M.
麦角酸二乙胺(LSD)是一种广泛使用的娱乐药物。本研究的目的是建立涡流LC-MS/MS法定量测定血清和尿液中的LSD及其主要代谢物2-氧代-3-羟基LSD(O-H-LSD)，无需耗时的提取步骤。该方法是在离子陷阱LC-MS/MS仪器上与湍流萃取系统耦合而成的。验证数据显示没有显著的基质效应，也没有观察到血清和尿液中的离子抑制。尿样和血清的平均日内精密度和准确度分别为101%和6.84%和97.40%和5.89%。O-H-LSD分别为97.50%和4.99%，血清为107%和4.70%。尿液和血清LSD的日间平均准确度和精密度分别为100%和8.26%，101%和6.56%。O-H-LSD在尿液和血清中分别为101%和8.11%，99.8%和8.35%。LSD的定量下限为0.1 ng/ml，血清LSD浓度可达8 ng/ml，尿液中2-氧-3-羟基LSD浓度可达250 ng/ml，在疑似LSD中毒患者的血药浓度和尿药浓度范围内，本方法准确、准确。到目前为止，该方法已应用于5例疑似LSD中毒患者，其中4次被证实服用了LSD，血清LSD浓度范围为1.80-14.70 ng/ml，1次尿液LSD浓度为1.25 ng/ml。2例患者血清中O-H-LSD浓度分别为0.99和0.45 ng/ml，1例患者尿中O-H-LSD浓度为9.70 ng/ml。
Lysergic acid diethylamide (LSD) is a widely used recreational drug. The aim of the present study is to develop a quantitative turboflow LC-MS/MS method that can be used for rapid quantification of LSD and its main metabolite 2-oxo-3-hydroxy LSD (O-H-LSD) in serum and urine in emergency toxicological cases without time-consuming extraction steps. The method was developed on an ion-trap LC-MS/MS instrument coupled to a turbulent-flow extraction system. The validation data showed no significant matrix effects and no ion suppression has been observed in serum and urine. Mean intraday accuracy and precision for LSD were 101 and 6.84 %, in urine samples and 97.40 and 5.89 % in serum, respectively. For O-H-LSD, the respective values were 97.50 and 4.99 % in urine and 107 and 4.70 % in serum. Mean interday accuracy and precision for LSD were 100 and 8.26 % in urine and 101 and 6.56 % in serum, respectively. For O-H-LSD, the respective values were 101 and 8.11 % in urine and 99.8 and 8.35 % in serum, respectively. The lower limit of quantification for LSD was determined to be 0.1 ng/ml. LSD concentrations in serum were expected to be up to 8 ng/ml. 2-Oxo-3-hydroxy LSD concentrations in urine up to 250 ng/ml. The new method was accurate and precise in the range of expected serum and urine concentrations in patients with a suspected LSD intoxication. Until now, the method has been applied in five cases with suspected LSD intoxication where the intake of the drug has been verified four times with LSD concentrations in serum in the range of 1.80-14.70 ng/ml and once with a LSD concentration of 1.25 ng/ml in urine. In serum of two patients, the O-H-LSD concentration was determined to be 0.99 and 0.45 ng/ml. In the urine of a third patient, the O-H-LSD concentration was 9.70 ng/ml.