Validation of an LC-MS/MS method for the quantitative analysis of 1P-LSD and its tentative metabolite LSD in fortified urine and serum samples including stability tests for 1P-LSD under different storage conditions

Jun 11, 2019Journal of pharmaceutical and biomedical analysis

Measuring 1P-LSD and its possible breakdown product LSD in urine and blood samples, including tests of 1P-LSD stability during storage

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Abstract

The limit of detection for 1-propionyl-LSD (1P-LSD) and LSD in serum and urine was established at 0.005 ng mL and 0.015 ng mL, respectively.

A highly sensitive method for quantifying 1P-LSD and LSD in biological samples using LC-MS/MS was developed and validated.
Stability tests indicated that 1P-LSD did not significantly degrade in urine and serum at -20 °C, 5 °C, or room temperature for up to five days.
LSD was found to degrade from 1P-LSD at room temperature, with hydrolysis observed in serum samples, reaching up to 21% conversion.
Sodium fluoride was effective in preventing the enzymatic conversion of 1P-LSD to LSD.
In an intoxication case, LSD was detected in urine and serum samples, while 1P-LSD was not detected, suggesting rapid hydrolysis in vivo.

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A variety of hallucinogens of the lysergamide type has emerged on the drug market in recent years and one such uncontrolled derivative of lysergic acid diethylamide (LSD) is 1-propionyl-LSD (1P-LSD). Due to the high potency of LSD and some of its derivatives (common doses: 50-200 μg), sensitive methods are required for the analysis of biological samples such as serum and urine. The occurrence of an intoxication case required the development of a fully validated, highly sensitive method for the quantification of 1P-LSD and LSD in urine and serum using LC-MS/MS. Given that LSD is unstable in biological samples when exposed to light or elevated temperatures, we also conducted stability tests for 1P-LSD in urine and serum under different storage conditions. The validation results revealed that the analysis method was accurate and precise with good linearity over a wide calibration range (0.015-0.4 ng mL). The limit of detection (LOD) and the lower limit of quantification (LLOQ) of 1P-LSD and LSD in serum and urine were 0.005 ng mLand 0.015 ng mL, respectively. The stability tests showed no major degradation of 1P-LSD in urine and serum stored at -20 °C, 5 °C or at room temperature for up to five days, regardless of protection from light. However, LSD was detected in all samples stored at room temperature showing a temperature-dependent hydrolysis of 1P-LSD to LSD to some extent (up to 21% in serum). Serum samples were particularly prone to hydrolysis possibly due to enzymatically catalyzed reactions. The addition of sodium fluoride prevented the enzymatic formation of LSD. The method was applied to samples obtained from the intoxication case involving 1P-LSD. The analysis uncovered 0.51 ng mLLSD in urine and 3.4 ng mLLSD in serum, whereas 1P-LSD remained undetected. So far pharmacokinetic data of 1P-LSD is missing, but with respect to the results of our stability tests and the investigated case rapid hydrolysis to LSD in-vivo seems more likely than instabilities of 1P-LSD in urine and serum samples. -1 -1 -1 -1 -1

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Validation of an LC-MS/MS method for the quantitative analysis of 1P-LSD and its tentative metabolite LSD in fortified urine and serum samples including stability tests for 1P-LSD under different storage conditions

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