氣相色譜-質(zhì)譜法同時分析運動營養(yǎng)品中的大麻酚、大麻二酚和Δ9-四氫大麻酚
發(fā)布時間:2018-04-18 18:39
本文選題:大麻酚 + 大麻二酚; 參考:《中國運動醫(yī)學雜志》2015年04期
【摘要】:目的:建立氣相色譜-質(zhì)譜法同時分析運動營養(yǎng)品中大麻酚、大麻二酚和Δ9-四氫大麻酚的檢測方法。方法:樣品采用液液萃取,提取液經(jīng)過正相固相萃取柱(Silica)純化,洗脫液氮氣吹干,N-甲基-N-(三甲基硅烷)三氟乙酰胺衍生化后,采用HP-1MS柱(17 m×0.2 mm i.d.×0.11 mm)色譜分離,程序升溫,質(zhì)譜檢測,D3-Δ9-四氫大麻酚為內(nèi)標。結果:大麻酚、大麻二酚和Δ9-四氫大麻酚的衍生化產(chǎn)物實現(xiàn)基線分離,三個定性特征離子的峰度比計算結果可以滿足世界反興奮劑機構(WADA)要求。該方法的檢測限為1μg/kg,定量限為2μg/kg,在添加的高、中、低三種濃度的相對回收率分布在94%~119%之間。結論:該方法滿足常規(guī)檢測要求,樣品前處理簡單、快速、可靠。
[Abstract]:Objective: to establish a gas chromatography-mass spectrometry method for simultaneous determination of cannabinol, cannabinol and 螖 9 tetrahydrocannabinol in sports nutrients.Methods: the sample was extracted by liquid-liquid extraction, the extract was purified by normal phase solid phase extraction column (Silica), and the eluate was dried by nitrogen. After derivatization of N-methyl-N-trifluoroacetamide, the chromatographic separation was performed on a HP-1MS column of 17 m 脳 0.2 mm i.d. 脳 0.11 mm.D3-螖 9-tetrahydrocannabinol was identified as internal standard by mass spectrometry.Results: the derivatization products of cannabinol, cannabinol and 螖 9-tetrahydrocannabinol were separated from baseline. The results of kurtosis ratio of the three qualitative characteristic ions could meet the requirements of the World Anti-Doping Agency (WADAA).The detection limit of the method is 1 渭 g / kg and the quantitative limit is 2 渭 g / kg. The relative recoveries of the three concentrations of high, middle and low concentrations are between 94g / kg and 119%.Conclusion: this method can meet the requirements of routine detection, and the sample pretreatment is simple, rapid and reliable.
【作者單位】: 國家體育總局反興奮劑中心食品藥品興奮劑檢測實驗室;
【分類號】:R155.5;O657.63
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