LC-ESI-MS/MS Simultaneous Analysis Method Coupled with Cation-Exchange Solid-Phase Extraction for Determination of Pyrrolizidine Alkaloids on Five Kinds of Herbal Medicines

Abstract

Background Pyrrolizidine alkaloids (PAs) are naturally occurring plant toxins associated with potential hepatic and carcinogenic diseases in humans and animals. The concern of PAs has been increased as the consumption of herbal medicines is increased. Objective This study aimed to develop and validate a sensitive analytical method to determine 28 PAs in 5 herbal medicines using liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS). Additionally, this study identified and quantified the amount of PA in 10 samples of each herbal medicine. Methods The pretreatment in the proposed LC-MS/MS analysis comprised solvent extraction using 0.05M H2SO4 in 50% methanol and clean-up step by MCX-solid-phase extraction (SPE) cartridge. The PA contents in herbal medicines were measured by using the developed method. Results The proposed method had recoveries ranged from 72.5% ∼ 123.7% for the Atractylodis Rhizoma Alba, 70.6% ∼ 151.7% for Alba Chrysanthmi Flos, 80.6% ∼ 130.9% for Leonuri Herba, 70.3% ∼ 122.9% for Gastrodiae Rhizoma, and 67.1% ∼ 106.9% for Glycyrrhizae Radix. Even though a few samples showed recoveries in unsatisfactory values, the proposed method indicated entirely sufficient recoveries and precisions in most samples. In monitoring results, only Leonuri Herba contained two PAs, which indicated Retrorsine (4/10) of 84.7 ∼ 120.9 μg/kg and Senkirkine (10/10) of 60.9 ∼ 170.7 μg/kg. Conclusions and Highlights As the proposed method is revealed to be a reliable procedure for monitoring 28 PAs in herbal medicines, it seems to contribute to controlling the risks coming from pyrrolizidine alkaloids in certain medicinal plants and dietary supplements.

An insight into recent updates on analytical techniques for bioactive alkaloids

“…The results revealed that the majority of herbal samples did not contain any of the 28 pyrrolizidine alkaloids. However, in the case of Leonuri Herba, retrorsine was identified within a concentration range of 84.7–120.9 μg/kg, and senkirkine was consistently present in all Leonuri Herba samples, with concentrations ranging from 60.9 to 170.7 μg/kg 96 …”

“…However, in the case of Leonuri Herba, retrorsine was identified within a concentration range of 84.7-120.9 μg/kg, and senkirkine was consistently present in all Leonuri Herba samples, with concentrations ranging from 60.9 to 170.7 μg/kg. 96 Pyrrolizidine alkaloids from herbal teas were detected using LC- 97 Klein and coworkers developed an LC-MS/MS method for the determination of pyrrolizidine alkaloids in cow milk samples. They extracted 51 pyrrolizidine alkaloids and two tropane alkaloids from 15 different cow milk samples.…”

GC-MS/MS Method for Determination of Polycyclic Aromatic Hydrocarbons in Herbal Medicines

“…That is, when there is a matrix effect, linearity should be evaluated using a standard solution containing the sample matrix [36]. Matrix effect can be classified as strong matrix effect below 50% or above 150%, moderate matrix effect between 50-80% or 120-150%, and low matrix effect between 80-120% [37]. Taking the criteria into account, the matrix effect on 8 PAHs was investigated.…”

“…The calibration curves were achieved from seven-point concentrations ranging from 1 to 100 ng/mL. The matrix effect was evaluated by the following formula [37]: Matrix effect (ME, %) = (slope of the calibration curve in matrix/slope of the calibration curve in solvent) × 100.…”

Solid-Phase Extraction and Characterization of Quercetrin-Rich Fraction from Melastoma malabathricum Leaves

“…The preconcentration-extraction-based techniques are still in significant use to make analytes available for sensitive measurements [11]. Among them, SPE is also frequently used to preconcentrate the target compound from plant materials that has been reported in many studies [12,13]. A small quantity of target compound from a highly complex phytochemical composition of plant samples could be preconcentrated prior to analytical determination [14].…”