Determination of Aconitum alkaloids in dietary supplements and raw botanical materials by liquid chromatography/UV detection with confirmation by liquid chromatography/tandem mass spectrometry: collaborative study.
An interlaboratory study was conducted to evaluate a method for the determination of 3 Aconitum alkaloids, viz., aconitine, mesaconitine, and hypaconitine, in raw botanical material and dietary supplements. The alkaloids were extracted with diethyl ether in the presence of ammonia. After cleanup by solid-phase extraction to remove matrix interferences, the alkaloids were determined by reversed-phase liquid chromatography (LC)/UV detection at 235 nm with confirmation by LC/tandem mass spectrometry (MS/MS). A total of 14 blind duplicates were successfully analyzed by 12 collaborators. For repeatability, the relative standard deviation (RSDr) values ranged from 1.9 to 16.7%, and for reproducibility, the RSDR values ranged from 6.5 to 33%. The HorRat values were all <2 with only one exception at 2.3. All collaborating laboratories had calibration curves with correlation coefficients of >0.998. In addition, 6 collaborators performed the confirmation and were able to verify the identities of the alkaloids by using LC/MS/MS.
Wong
Siu-Kay
SK
Hong Kong Government Laboratory, 88 Chung Hau St, Homantin, Hong Kong SAR, China. skwong@govtlab.gov.hk
D031841:Aconitum / Q000737:chemistry*; D000470:Alkaloids / Q000032:analysis* / Q000737:chemistry / Q000302:isolation & purification; D002853:Chromatography, Liquid / Q000379:methods; D019587:Dietary Supplements; D007202:Indicators and Reagents; D012680:Sensitivity and Specificity; D013056:Spectrophotometry, Ultraviolet / Q000379:methods; D053719:Tandem Mass Spectrometry / Q000379:methods
D000470:Alkaloids; D007202:Indicators and Reagents