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.
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.
Department of Analytical Chemistry, School of Pharmacy, Shenyang Pharmaceutical University, 103 Wenhua Road, Shenyang 110016, China.
Ning
N
Li
Mei
M
Cui
Xiumei
X
Lu
Feng
F
Qin
Kun
K
Jiang
Famei
F
Li
D002681:China; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D019587:Dietary Supplements / Q000032:analysis*; D004340:Drug Contamination; D004365:Drugs, Chinese Herbal / Q000032:analysis*; D007004:Hypoglycemic Agents / Q000032:analysis* / Q000138:chemical synthesis; D053719:Tandem Mass Spectrometry / Q000379:methods*
D004365:Drugs, Chinese Herbal; D007004:Hypoglycemic Agents