Method for the Simultaneous Determination of<i>Aconitum</i>Alkaloids and their Hydrolysis Products by Gas Chromatography-Mass Spectrometry in Human Serum

Ito, Kitae; Ohyama, Yoshiharu; Konishi, Yuko; Tanaka, Satoshi; Mizugaki, Michinao

doi:10.1055/s-2006-957609

Cited by 36 publications

(25 citation statements)

References 3 publications

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“…For the analysis of the Aconitum alkaloids in biological specimens such as blood, serum and urine, several GC-MS methods have been described [12,18,21,28,29]. These employ a variety of extraction procedures followed by derivatisation to their TMS derivatives.…”

Section: Introductionmentioning

confidence: 99%

Determination of aconitine in body fluids by LC-MS-MS

et al. 2004

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A very sensitive and specific method was developed for the determination of aconitine, the main toxic alkaloid from plants of the genus Aconitum L., in biological samples. The method comprised solid-phase extraction using mixed-mode Cs cation exchange columns followed by liquid chromatography-tandem mass spectrometry (LC-MS-MS). Chromatographic separation was achieved with a RP8 column. Detection of aconitine was achieved using electrospray in the positive ionisation mode and quantification was performed using multiple reaction monitoring with m/z 646.4 as precursor ion, i.e. [M+H]+ of aconitine and m/z 586.5, m/z 526.4 and m/z 368.4 as product ions after collision-induced dissociation. The method was fully validated for the analysis of blood samples: the limit of detection and the limit of quantitation were 0.1 ng/g and 0.5 ng/g, respectively. Within the linear calibration range of 0.5-25 ng/g, analytical recovery was 79.9%. In two fatal cases with suspected aconite intoxication, aconitine could be detected in blood samples at concentrations of 10.0 and 12.1 ng/g. In one case, aconitine could also be detected in the stomach content (3 ng/g) and in the other in the urine (180 ng/ml).

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Section: Introductionmentioning

confidence: 99%

Determination of aconitine in body fluids by LC-MS-MS

et al. 2004

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“…To utilize this herbal medicine safely, it is urgent to develop a simple, fast and efficient method for simultaneous determination of these three alkaloids. Among the analytical techniques, GC/MS [7,8], HPLC [9,10] and CE [11,12], have been used for the determination of these three alkaloids. However, CE is getting more frequently used owing to its inherent high separation efficiency and simplicity of instruments.…”

Section: Introductionmentioning

confidence: 99%

CE‐electrochemiluminescence with ionic liquid for the facile separation and determination of diester‐diterpenoid aconitum alkaloids in traditional Chinese herbal medicine

Bao

Yang

2011

Electrophoresis

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A CE-electrochemiluminescence(CE-ECL) detection system, CE/tris(2,2'-bipyridyl) ruthenium(II)ECL with ionic liquid, was established for the determination of diester-diterpenoid aconitum alkaloids (aconitine (AC), mesaconitine (MA) and hypaconitine (HA)) in traditional Chinese herbal medicine. Running buffer containing 25 mM borax-20 mM 1-ethyl-3-methylimidazolium tetrafluoroborate at pH 9.15 was used, which resulted in significant changes in separation and obvious enhancement in ECL intensity for AC, MA and HA with similar structures. End-column detection was achieved in 50 mM phosphate buffer with 5 mM Ru(bpy)₃²⁺ (pH 9.15) at applied detection voltage of 1.20 V when the distance between the Pt working electrode and outlet of capillary (50 cm × 25 μm id) was set at 150 μm. One single quantitative analysis of three alkaloids was achieved at a separation voltage of 15 kV within 10 min. Moreover, two extraction processes (ethanol extraction and ethyl ether extraction after basification) were investigated. The result showed that ethanol extraction process has higher extraction efficiency than ethyl ether extraction process. Under the optimized conditions, the detection limits of AC, MA and HA were 5.62 × 10(-8) , 2.78 × 10(-8) and 3.50 × 10(-9) mol/L (S/N=3), respectively. The method was successfully applied to determine the amounts of AC, MA and HA in the aconitum herbal samples.

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“…in blood or urine [4][5][6][7]. Gas chromatography (GC) with MS detection that needed tedious derivatization has also been reported [8]. But none of the above methods were validated for the pharmacokinetic study in humans.…”

Section: Introductionmentioning

confidence: 99%