首页> 外文期刊>Journal of chromatography, B. Analytical technologies in the biomedical and life sciences >Simultaneous detection of 22 toxic plant alkaloids (aconitum alkaloids, solanaceous tropane alkaloids, sophora alkaloids, strychnos alkaloids and colchicine) in human urine and herbal samples using liquid chromatography-tandem mass spectrometry
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Simultaneous detection of 22 toxic plant alkaloids (aconitum alkaloids, solanaceous tropane alkaloids, sophora alkaloids, strychnos alkaloids and colchicine) in human urine and herbal samples using liquid chromatography-tandem mass spectrometry

机译:使用液相色谱-串联质谱法同时检测人尿液和草药样品中的22种有毒植物生物碱(芦荟生物碱,茄碱托烷生物碱,槐属生物碱,兜兰生物碱和秋水仙碱)

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摘要

A liquid chromatography-tandem mass spectrometry method for simultaneous detection of 22 toxic plant alkaloids, including aconitum alkaloids and their hydrolyzed products (aconitine, hypaconitine, mesaconitine, yunaconitine, crassicauline A, benzoylaconine, benzoylmesaconine, benzoylhypaconine, deacetylyunaconitine, deacetylcrassicauline A), solanaceous tropane alkaloids (atropine, anisodamine, scopolamine, anisodine), sophora alkaloids (matrine, sophoridine, oxymatrine, cytisine, N-methylcytisine), strychnos alkaloids (brucine, strychnine) and colchicine, in herbal and urine samples was developed and validated. Following sample preparation by liquid-liquid extraction, chromatographic separation was achieved on Eclipse XDB C8 column. Identification was based on two multiple reaction monitoring transitions and the relative ion intensity. Method selectivity was demonstrated. The limits of detection were 5. ng/mL for all analytes, except 50. ng/mL for cytisine. The herbal matrix effects ranged from 89% to 118%, whereas the urine matrix effects were between 91% and 109% for all analytes except cytisine (57%) and N-methylcytisine (67%). The urine extraction recovery ranged from 74% to 110% for all analytes, except cytisine (15%) and oxymatrine (30%). With the good extraction efficiency of the other major sophora alkaloids, the relatively low extraction recovery of the minor sophora alkaloids cytisine and oxymatrine did not affect identification of sophora alkaloids as a group. Carry-over was minimal at less than 0.1%. The method was successfully applied in analysis of 170 cases of suspected herbal poisoning, with aconitum alkaloids, sophora alkaloids, solanaceous tropane alkaloids, and strychnos alkaloids being detected in 53, 42, 18, and 6 cases, respectively.
机译:液相色谱-串联质谱法同时检测22种有毒植物生物碱,包括乌头生物碱及其水解产物(aco碱,扁豆碱,中aco碱,芸豆碱,角ass碱A,苯甲酰可卡因,苯甲酰基美甲con碱,苯甲酰高pa碱,去乙酰基菜碱,去乙酰基yun碱已开发并验证了草药和尿液样品中的生物碱(阿托品,山iso碱,东pol碱,东pol碱,山iso碱),槐属生物碱(苦参碱,槐定碱,氧化苦参碱,胱氨酸,N-甲基胞嘧啶碱),马钱子碱生物碱(芥子碱,士丁宁)和秋水仙碱。通过液-液萃取制备样品后,在Eclipse XDB C8色谱柱上进行色谱分离。鉴定基于两个多重反应监测过渡和相对离子强度。证明了方法的选择性。对于所有分析物,检测限为5. ng / mL,对胱氨酸的检测限为50. ng / mL。除胱氨酸(57%)和N-甲基胱氨酸(67%)外,所有分析物的草药基质效应范围从89%至118%,而尿基质效应介于91%至109%之间。除胱氨酸(15%)和氧化苦参碱(30%)外,所有分析物的尿液提取回收率在74%至110%之间。由于其他主要槐花生物碱具有良好的提取效率,次要槐花生物碱胱氨酸和氧化苦参碱的提取回收率较低,因此不会影响槐花生物碱的整体鉴定。残留量最小,不到0.1%。该方法已成功地用于170例可疑草药中毒的分析中,乌头生物碱,槐属生物碱,茄碱托烷生物碱和马兜铃生物碱分别检出53、42、18和6例。

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