Simultaneous Determination of Statins in Dietary Supplements by Ultra-Performance Liquid Chromatography

Abstract

A method for the determination of 12 statins [atorvastatin ATOR , cerivastatin CERI , fluvastatin FLU , lovastatin LO , lovastatin acid LOA , mevastatin ME , mevastatin acid MEA , pitavastatin PITA , pravastatin PRA , rosuvastatin ROSU , simvastatin SIM , and simvastatin acid SIMA ] in dietary supplements by ultra-performance liquid chromatography UPLC has been developed. Statins were ultrasonically extracted with 50 v/v methanol. Clean-up was performed using an Oasis MAX mini-cartridge column with methanol and methanol containing 0.2 v/v phosphoric acid as an eluting solvent. UPLC separation was performed on an ACQUITY UPLC BEH C18 column 2.1 mm i.d. 150 mm, 1.7 μm with 0.2 v/v phosphoric acid aqueous solutionacetonitrile gradient. The method was validated for dietary supplements spiked with the 12 statins at the quantitation limits and 10 times the quantitation limits, and the recoveries of statins were between 89.2 and 100.9 . Relative standard deviation values of repeatability and intermediate precision were not more than 7 . The analytical method was applied to 24 commercial dietary supplements. LO and LOA were found at maximum concentrations of 4.85 mg/packet and 1.28 mg/capsule, respectively. Other statins were not detected. When a dietary supplement was consumed according to the directions on the package, the daily intake of LO was 6.74 mg. This could be dangerous to consumers because it exceeds one half of the lowest recommended daily dose of LO 10 mg .

An in vitro evaluation of the effects of different statins on the structure and function of human gut bacterial community

“…Statin was dissolved in 50% DMSO-50% water (v/v) and added to the medium to obtain a final statin concentration of 20 μM or colon concentration [23]; controls were added with 50% DMSO only (all samples content 1% DMSO finally). The colon concentrations of ROS, SIM, FLU, and ATO were set at the dose of 10 mg, 20 mg, 80 mg, and 20 mg per day [24], which is about 30, 40, 240, and 64 μg/mL in vitro, and we detected the concentrations at 0 h to establish a baseline (28,33,265, and 82 μg/mL, respectively). The filtered fresh fecal slurry (500 μL) was added to the previously prepared fermentation culture medium (9.5 mL), within an anaerobic chamber, and then incubated at 37˚C.…”

“…Statins were analyzed by the Shimadzu Black 20 AT system (Shimadzu, Kyoto, Japan) as previously described [32,33] with some modifications. Briefly, statin fermentation samples were just centrifuged (14,000 g for 20 min), and the supernatant was used for statin analysis by HPLC.…”

Simultaneous screening of dietary supplements for 25 anti‐hyperlipidemic substances using ultra‐performance liquid chromatography and liquid chromatography/electrospray ionization tandem mass spectrometry

“…Common adulterants include erectile dysfunction, anti‐hypertensive, anti‐diabetic, and anti‐obesity drugs 10–13 . In addition, in recent years, lovastatin, lovastatin acid and bezafibrate have been found unexpectedly in red yeast rice supplements 14–16 . This adulteration presents a serious threat to consumer health because of a lack of data or inaccurate safety data, as well as the potential for undesirable side effects 16,17 .…”

Assay of lovastatin containing dietary supplement by LC‐MS/MS under MRM condition

“…Several analytical methods report the quantitative determination of lovastatin in different matrices. Different approaches and sample preparation protocols are used; the assays are based on HPLC, gas chromatography, electrochemical analysis, and MS . Mass spectrometry is a remarkably sensitive and specific analytical instrumentation that can both determine the structure and the amount of analytes within a sample .…”

“…Several analytical methods report the quantitative determination of lovastatin in different matrices. Different approaches and sample preparation protocols are used; the assays are based on HPLC, gas chromatography, electrochemical analysis, and MS. [22][23][24][25][26][27][28][29][30][31][32][33][34] Mass spectrometry is a remarkably sensitive and specific analytical instrumentation that can both determine the structure and the amount of analytes within a sample. [35][36][37] In particular, electrospray ionization (ESI) MS is 1 of the most versatile ion sources used in a wide range of analytical applications; moreover, the MRM analysis mode is a targeted mass spectrometry approach that has being used for decades for accurate quantification of small molecules in complex matrices.…”