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经曼陀罗慢性暴露后,采用 LC-MS/MS 法测定毛发中的阿托品和东莨菪碱。

Measurement of atropine and scopolamine in hair by LC-MS/MS after Datura stramonium chronic exposure.

机构信息

Laboratory of Pharmacology-Toxicology, AP-HP, Raymond Poincaré Universitary Hospital, Versailles Saint Quentin-en-Yvelines University, 104 Boulevard Raymond Poincaré, 92380 Garches, France.

出版信息

Forensic Sci Int. 2012 Nov 30;223(1-3):256-60. doi: 10.1016/j.forsciint.2012.09.015. Epub 2012 Oct 22.

Abstract

BACKGROUND

Datura stramonium is an herbaceous annual plant. All parts of the plant contain tropane alkaloids such as atropine and scopolamine. We report the case of a 22-year-old man admitted to a general hospital for visual and aural hallucinations. One week after his admission, as the hallucinations remained, the patient was transferred to a psychiatric hospital. Neither blood nor urine was conserved during his hospitalization, so a hair analysis was requested in order to identify a possible consumption of a Datura seed infusion.

METHODS

After decontamination and washing, hair strands were segmented into four pieces and grinded into a fine and homogeneous powder. We then incubated 20 mg for 10 min in 1 mL of phosphate buffer at pH 5.0 in the presence of 100 ng of ketamine-d4, used as internal standard (IS). Liquid-liquid extraction was performed with 4 mL of a mixture of hexane/ethyl acetate (1/1, v/v). The residue was reconstituted in 80 μL of mobile phase. A further 10 μL were injected into an 1.9 μm Hypersil GOLD PFP column (100 mm×2.1 mm) eluted with a gradient of acetonitrile and 2 mmol/L 0.1% formate buffer at a flow rate of 300 μL/min. Compounds were detected by a LCQ TSQ Vantage XP triple-quadripole mass spectrometer equipped with an electrospray ionization (ESI) source set in positive mode. SRM transitions m/z 290.2→124.1, m/z 304.2→138.1, and m/z 242.1→129.1 were optimized for atropine, scopolamine and IS, respectively.

RESULTS

The assay was accurate and precise over the range of 1.0 (lower limit of quantification) to 1000.0 pg/mg (upper limit of quantification) in hair. Both atropine (from 8.4 to 15.0 pg/mg) and scopolamine (1.0-1.3 pg/mg) were identified in the four segment of the hair showing a regular consumption of Datura admitted by the patient himself.

CONCLUSION

We report here the first description of atropine with scopolamine in a Caucasian dark man's hair after D. stramonium chronic exposure, using a validated LC-MS/MS method.

摘要

背景

曼陀罗是一种一年生草本植物。植物的所有部分都含有托烷生物碱,如阿托品和东莨菪碱。我们报告了一例 22 岁男性因视觉和听觉幻觉入院的病例。入院一周后,由于幻觉持续存在,患者被转至精神病院。患者住院期间未保留血样和尿样,因此要求进行毛发分析,以确定是否摄入了曼陀罗种子浸液。

方法

在去污和洗涤后,将毛发分成 4 段并研磨成细而均匀的粉末。然后,我们将 20mg 粉末在 pH 5.0 的磷酸盐缓冲液中孵育 10 分钟,同时加入 100ng 的酮咯酸-d4(用作内标)。采用正相固相萃取法提取 4mL 己烷/乙酸乙酯(1/1,v/v)混合物。残渣用 80μL 流动相重新溶解。进一步取 10μL 注入 1.9μm Hypersil GOLD PFP 柱(100mm×2.1mm),以乙腈和 2mmol/L 0.1%甲酸缓冲液为流动相进行梯度洗脱,流速为 300μL/min。采用电喷雾电离源(ESI)在正模式下,将化合物检测到 LCQ TSQ Vantage XP 三重四极杆质谱仪。优化了 290.2→124.1、304.2→138.1 和 242.1→129.1 的 SRM 跃迁,用于阿托品、东莨菪碱和内标。

结果

在毛发中,检测范围为 1.0(定量下限)至 1000.0pg/mg(定量上限),该方法准确且精密。在毛发的四个部位均检测到了阿托品(8.4-15.0pg/mg)和东莨菪碱(1.0-1.3pg/mg),这表明患者确实有规律地摄入了曼陀罗。

结论

我们在此报告了首例使用 LC-MS/MS 方法在一名白人深色男子的毛发中检测到阿托品和东莨菪碱的案例,该男子曾有过慢性接触曼陀罗的经历。

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