Method For Determination Of Alkaloids Research Articles

Simultaneous determination of 16 alkaloids in blood by ultrahigh-performance liquid chromatography-tandem mass spectrometry coupled with supported liquid extraction

Alkaloids are widely present in food and medicine. However, many alkaloids have poisoning effect. Thus, a sensitive and rapid method for determination of alkaloids is highly desired. In this study, a convenient, reliable and accurate method is developed for the simultaneous determination of 16 poisonous alkaloids in human blood by ultrahigh performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) coupled with supported liquid extraction (SLE). The 16 alkaloids include colchicine, anisodamine, scopolamine, atropine, sinomenine, dicaine, thebaine, papaverine, strychnine, brucine, aconitine, hypaconitine, yunaconitine, deoxyaconitine, bullatine A and bullatine B. Low limits of detection (LODs) were obtained ranging in 0.002–0.03 μg L−1. The linear ranges are 0.005–200 μg L−1 for colchicine, papaverine, brucine, aconitine, hypaconitine, yunaconitine and deoxyaconitine, 0.01–200 μg L−1 for anisodamine and scopolamine, 0.05–200 μg L−1 for atropine, strychnine, bullatine A and bullatine B, 0. 1–200 μg L−1 for other target analytes, all with correlation coefficients (R2) higher than 0.995. The recoveries range from 79.2% to 95.8%. The relative standard deviation (RSD) values are lower than 15% and the values of matrix effect (ME) range in 86.3%–118.2%. This method of UPLC−MS/MS coupled with SLE has high potential for analyzing multiple alkaloids in blood samples.

Development and Validation of a Reversed-Phase HPLC Method for Determination of Alkaloids from Papaver somniferum L. (Papaveraceae)

An HPLC method for the separation of six target alkaloids from Papaver somniferum L. (morphine, codeine, oripavine, thebaine, papaverine, and noscapine) was developed, optimized, and validated. The chromatographic behavior of these alkaloids was investigated using a reversed-phase chromatography at acidic and alkaline pH. The effects of ion-pairing agents, pH value of the mobile phase, concentration of the buffer components, mobile phase organic modifier, and column temperature were studied. Regardless of the large differences in their pKa values, all alkaloids were separated within a close retention window, and good peak shape was achieved for each of the six alkaloids. The proposed method has adequate selectivity, linearity, accuracy, precision, and reproducibility and is applicable for poppy straw.

Rapid discrimination and quantification of alkaloids in Corydalis Tuber by near-infrared spectroscopy

With the application of near-infrared spectroscopy (NIRS), a convenient and rapid method for determination of alkaloids in Corydalis Tuber extract and classification for samples from different locations have been developed. Five different samples were collected according to their geographical origin, 2-Der with smoothing point of 17 was applied as the spectral pre-treatment, and the 1st to scaling range algorithm was adjusted to be optimal approach, classification model was constructed over the wavelength range of 4582–4270 cm −1, 5562–4976 cm −1 and 7000–7467 cm −1 with a great recognition rate. For prediction model, partial least squares (PLS) algorithm was utilized referring to HPLC-UV reference method, the optimum models were obtained after adjustment. Pre-processing methods of calibration models were COE for protopine and min–max normalization for palmatine and MSC for tetrahydropalmatine, respectively. The root mean square errors of cross-validation (RMSECV) for protopine, palmatine, tetrahydropalmatine were 0.884, 1.83, 3.23 mg/g. The correlation coefficients ( R 2) were 99.75, 98.41 and 97.34%. T test was applied, in the model of tetrahydropalmatine; there is no significant difference between NIR prediction and HPLC reference method at 95% confidence interval with t = 0.746 < t (0.05,20) = 2.086, therefore NIRS is a reliable analytical tool in establishing prediction models.