Abstract:

An analytical method was developed for simultaneous rapid determination of 12 anti-allergic chemical drugs in Chinese traditional patent medicine and health food by supercritical fluid chromatography tandem mass spectrometry with solid phase extraction (SPE-SFC-MS/MS). Samples were extracted with methanol by sonification and then purified by Oasis mixed-model cation exchange SPE. The extracts were separated on a Waters Trefoil CEL1 (150 mm×3.0 mm, 2.5 μ m) column with a mobile phase consisting of carbon dioxide-methanol containing 0.1% (v/v) ammonia water in a gradient elution mode, at a flow rate of 1.2 mL/min. The column temperature was 45℃ and the back pressure was 12.4×10⁶ Pa. The whole analysis was completed in 10 min. The 12 anti-allergic chemical drugs were detected by an electrospray ion source in positive or negative modes with a multiple reaction monitoring (MRM) mode. The calibration curves of the 12 anti-allergic chemical drugs showed good linearities in the range of 5-250 μ g/L with the correlation coefficients (r) ≥ 0.998. The limits of detection (LODs) were 0.141-0.262 μ g/L, and the limits of quantification (LOQs) were 0.703-1.308 μ g/L. The recoveries of the 12 anti-allergic chemical drugs at spiked levels of 10, 20 and 100 μ g/L were in the range of 76.1%-112.5%, and the relative standard deviations (RSDs) were 1.1%-8.3% (n=6). The method is simple, sensitive and reliable. It has been successfully used for the detection of illegally added anti-allergic chemical drugs in Chinese traditional patent medicine and health food.

Key words: anti-allergic chemical drug, Chinese traditional patent medicine, health food, mass spectrometry (MS), solid phase extraction (SPE), supercritical fluid chromatography (SFC)