Abstract：
BACKGROUND: Ayahuasca is a psychoactive drink originally consumed by indigenous people of the Amazon. The lack of regulation of this drink leads to uncontrolled consumption, and it is often consumed in religious contexts.
OBJECTIVE: The aim of this work is to compare three miniaturised extraction techniques for extracting the main ayahuasca compounds from beverages.
METHODS: Three sample pretreatment techniques were evaluated (dispersive liquid-liquid microextraction [DLLME], microextraction by packed sorbent [MEPS] and QuEChERS [Quick, Easy, Cheap, Effective, Rugged and Safe]) for the simultaneous extraction of N,N-dimethyltryptamine (DMT), tetrahydroharmine (THH), harmine, harmaline, harmol and harmalol from ayahuasca beverage samples. Then, the most promising technique (QuEChERS) was chosen to pre-concentrate the analytes, subsequently detected by high-performance liquid chromatography coupled to a diode array detector (HPLC-DAD).
RESULTS: The procedure was optimised, with the final conditions being 500 μL of extractor solvent, 85 mg of primary secondary amine (PSA) and 4 s of vortexing. The analytical method was validated, showing to be linear between 0.16 and 10 μg/mL for β-carbolines and between 0.016 and 1 μg/mL for DMT, with coefficients of determination (R2) between 0.9968 and 0.9993. The limit of detection (LOD) and lower limit of quantification (LLOQ) were 0.16 μg/mL for all compounds, except for DMT (0.016 μg/mL) and extraction efficiencies varied between 60.2% and 88.0%.
CONCLUSIONS: The analytical methodology proved to be accurate and precise, with good linearity, LODs and LLOQs. This method has been fully validated and successfully applied to ayahuasca beverage samples.
OBJECTIVE: The aim of this work is to compare three miniaturised extraction techniques for extracting the main ayahuasca compounds from beverages.
METHODS: Three sample pretreatment techniques were evaluated (dispersive liquid-liquid microextraction [DLLME], microextraction by packed sorbent [MEPS] and QuEChERS [Quick, Easy, Cheap, Effective, Rugged and Safe]) for the simultaneous extraction of N,N-dimethyltryptamine (DMT), tetrahydroharmine (THH), harmine, harmaline, harmol and harmalol from ayahuasca beverage samples. Then, the most promising technique (QuEChERS) was chosen to pre-concentrate the analytes, subsequently detected by high-performance liquid chromatography coupled to a diode array detector (HPLC-DAD).
RESULTS: The procedure was optimised, with the final conditions being 500 μL of extractor solvent, 85 mg of primary secondary amine (PSA) and 4 s of vortexing. The analytical method was validated, showing to be linear between 0.16 and 10 μg/mL for β-carbolines and between 0.016 and 1 μg/mL for DMT, with coefficients of determination (R2) between 0.9968 and 0.9993. The limit of detection (LOD) and lower limit of quantification (LLOQ) were 0.16 μg/mL for all compounds, except for DMT (0.016 μg/mL) and extraction efficiencies varied between 60.2% and 88.0%.
CONCLUSIONS: The analytical methodology proved to be accurate and precise, with good linearity, LODs and LLOQs. This method has been fully validated and successfully applied to ayahuasca beverage samples.
摘要：
背景：Ayahuasca是一种精神活性饮料，最初由亚马逊土著居民食用。这种饮料缺乏监管导致不受控制的消费，它经常在宗教环境中消费。
目的：这项工作的目的是比较三种小型化提取技术，用于从饮料中提取主要的ayahuasca化合物。
方法：评估了三种样品预处理技术（分散液液微萃取[DLLME]，通过填充吸附剂[MEPS]和QuEChERS进行微萃取[快速，Easy,便宜,有效,坚固且安全])用于同时提取N，N-二甲基色胺(DMT),四氢harmine(THH),Harmine,Harmaline,来自ayahuasca饮料样品的harmol和harmalol。然后，选择最有前途的技术（QuEChERS）来预先浓缩分析物，随后通过与二极管阵列检测器（HPLC-DAD）耦合的高效液相色谱进行检测。
结果：优化了程序，最终条件为500μL提取溶剂，85毫克的伯仲胺（PSA）和4秒的涡旋。对分析方法进行了验证，β-咔啉在0.16至10μg/mL之间呈线性关系，DMT在0.016至1μg/mL之间呈线性关系，决定系数(R2)在0.9968和0.9993之间。所有化合物的检出限（LOD）和定量下限（LLOQ）均为0.16μg/mL，除DMT（0.016μg/mL）外，提取效率在60.2％至88.0％之间变化。
结论：分析方法被证明是准确和精确的，具有良好的线性度，LOD和LLOQ。该方法已得到充分验证，并成功应用于ayahuasca饮料样品。
目的：这项工作的目的是比较三种小型化提取技术，用于从饮料中提取主要的ayahuasca化合物。
方法：评估了三种样品预处理技术（分散液液微萃取[DLLME]，通过填充吸附剂[MEPS]和QuEChERS进行微萃取[快速，Easy,便宜,有效,坚固且安全])用于同时提取N，N-二甲基色胺(DMT),四氢harmine(THH),Harmine,Harmaline,来自ayahuasca饮料样品的harmol和harmalol。然后，选择最有前途的技术（QuEChERS）来预先浓缩分析物，随后通过与二极管阵列检测器（HPLC-DAD）耦合的高效液相色谱进行检测。
结果：优化了程序，最终条件为500μL提取溶剂，85毫克的伯仲胺（PSA）和4秒的涡旋。对分析方法进行了验证，β-咔啉在0.16至10μg/mL之间呈线性关系，DMT在0.016至1μg/mL之间呈线性关系，决定系数(R2)在0.9968和0.9993之间。所有化合物的检出限（LOD）和定量下限（LLOQ）均为0.16μg/mL，除DMT（0.016μg/mL）外，提取效率在60.2％至88.0％之间变化。
结论：分析方法被证明是准确和精确的，具有良好的线性度，LOD和LLOQ。该方法已得到充分验证，并成功应用于ayahuasca饮料样品。
