Detection and characterization of synthetic steroidal and non-steroidal anti-inflammatory drugs in Indian ayurvedic/herbal products using LC-MS/TOF

• Published in: Drug testing and analysis 2009-08, Vol.1 (8), p.372-381
• Main Authors: Savaliya, Akash A., Prasad, Bhagwat, Raijada, Dhara K., Singh, Saranjit
• Format: Article
• Language: English
• Subjects: adulteration; Anti-Inflammatory Agents - analysis; Anti-Inflammatory Agents - isolation & purification; Anti-Inflammatory Agents, Non-Steroidal - analysis; Anti-Inflammatory Agents, Non-Steroidal - isolation & purification; Ayurvedic/herbal healthcare products; Chromatography, High Pressure Liquid - methods; Drug Contamination; India; LC-MS/TOF; non-steroidal anti-inflammatory drugs steroids; Plant Preparations - chemistry; Spectrometry, Mass, Electrospray Ionization - economics; Spectrometry, Mass, Electrospray Ionization - methods; Steroids - isolation & purification
• ISSN: 1942-7603; 1942-7611
• DOI: 10.1002/dta.75

It is claimed that ayurvedic/herbal healthcare products (AHPs) are safe because of their natural origin. However, several reports exist of adulteration of AHPs with synthetic drugs. In this study, a generalized strategy was developed using LC‐MS/TOF for the detection and verification of steroidal and anti‐inflammatory drugs in 58 AHPs collected from various parts of India. The strategy involved recording of mass spectral information for standard drugs—including ionization mode (ESI/APCI − ve or + ve), mass spectrum, accurate mass, identification of qualifier fragments (two), extracted ion chromatograms (EICs), isotopic pattern and determination of UV max (nm)—through UV‐PDA studies. Adulteration was then detected in AHPs primarily through comparison of EICs at accurate m/z for molecular ion peaks and RT matching with the standard. It was confirmed by spiking with the standards, and matching mass spectrum, accurate mass, RT of qualifier fragments, isotopic pattern and UV spectrum of the standards with the adulterant peaks in AHPs. Dexamethasone and diclofenac were detected as adulterants in ten AHPs whereas one AHP tested positive for piroxicam and another for dexamethasone. All the adulterated products were sold by the healthcare practitioners, while no product marketed by manufacturers or chemist shops had this problem. The study showed that LC‐MS/TOF‐based screening could be used as a rapid approach to monitor adulteration of steroids and anti‐inflammatory drugs in AHPs. Copyright © 2009 John Wiley & Sons, Ltd. A novel and simple EIC‐based LC‐MS/TOF approach was developed and employed for the determination of adulteration of synthetic steroidal and non‐steroidal anti‐inflammatory drugs in Indian ayurvedic herbal products. Of the total 58 products tested, none of the marketed product had any tested adulterant, while 12 products sold by the practitioners were adulterated with dexamethasone, diclofenac and/or piroxicam.