A rapid and reliable UPLC‐MS/MS method for the identification and quantification of fourteen synthetic anti‐diabetic drugs in adulterated Chinese proprietary medicines and dietary supplements

Abstract

An ultraperformance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for simultaneous qualitative and quantitative analysis of 14 synthetic anti-diabetic drugs in adulterated Chinese proprietary medicines (CPMs) and dietary supplements. The samples were prepared by ultrasonic extraction with methanol and separated on a C₁₈ column with mobile phase consisting of acetonitrile and water (both containing 0.10% formic acid). Gradient elution was applied with a flow rate of 0.20 mL/min. Two transitions from protonated molecules were monitored for each synthetic anti-diabetic drug in positive mode of electrospray ionization (ESI). The two transitions, the peak area ratio of the two transitions and the retention time were used for identification. The more intensive transition was used for quantification. The analysis time was 6 min per sample. Satisfactory linear relationships were estimated between the peak area and the concentration with correlation coefficients higher than 0.995. The limit of detection ranged from 0.03 to 5.45 ng/mL. The relative standard deviation of intra-day precision was below 7.6%, the RSD of inter-day precision was below 15% and the relative error of accuracy was between -10 and 7.8%. The proposed method is rapid, selective, reliable and was successfully applied to the analysis of 30 real samples of 22 CPMs and eight dietary supplements from the local market in China.

Validation of an LC–MS/MS method for analysis of anti‐diabetic drugs in botanical dietary supplements labeled for blood sugar management

“…When comparing our method with previously published methods for analysis of anti‐diabetic compounds in botanical dietary supplements, we note that our method provides adequate selectivity, sensitivity, accuracy, and precision and simultaneously analyzes a wider range of target compounds including anti‐diabetic, anti‐obesity, and cholesterol‐lowering compounds. However, the instrument was not run in full scan mode and therefore, would not likely detect any adulterants other than the 19 targeted analytes.…”

“…The selectivity of the method was investigated by comparing the LC–MS/MS chromatograms of the blank matrix extract with those of the blank matrix extract spiked with 19 target analytes. Matrix effects were measured for each standard at 25, 100, and 400 ng/mL in methanol and compared to a post‐extraction fortified matrix …”

“…The presence of synthetic anti‐diabetic drugs (eg, metformin, phenformin, rosiglitazone, gliclazide, glibenclamide, glimepiride) in Chinese proprietary medicines, anti‐diabetic herbal medicines, and products identified as dietary supplements and labeled for blood sugar management is well documented . A variety of analytical methods has been developed for detecting synthetic drugs in traditional herbal medicines and these reports are usually accompanied by analyses of proprietary medicines or dietary supplements sold for blood sugar management . [Table S1 (Supporting Information)].…”

Study on the hypoglycemic activities and metabolism of alcohol extract of Alismatis Rhizoma

“…Traditional medicine is a fruitful source of future drugs to counteract insulin resistance, consistent with a resurgence of interest in drug discovery from natural products [12][13][14]. Alismatis rhizome (Zexie in Chinese), one of the commonly used traditional Chinese medicines, is derived from the dried rhizomes of Alisma orientale (Sam.)…”

Analysis of Drugs Illegally Added into Chinese Traditional Patent Medicine Using Surface-enhanced Raman Scattering

“…The main methods for these detections include thin-layer chromatography (TLC), 10 high-performance liquid chromatography (HPLC), 11,12 liquid chromatography-mass spectrometry (LC-MS), 9,13,14 ultra-performance liquid chromatography-mass spectrometry (UPLC-MS-MS), 15 TLC-MS, 16 and GC-MS. 17 These methods can provide results with high accuracy and reliability, but almost all require a cumbersome pretreatment and a time-consuming procedure. The instruments are expensive and the experimental conditions are rigorous.…”