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. 2016 May-Jun;54(5):847-57.
doi: 10.1093/chromsci/bmv246. Epub 2016 Feb 4.

Multiwalled Carbon Nanotubes-Dispersive Solid-Phase Extraction Coupled with UPLC-ESI-MS-MS for Simultaneous Determination of 10 Illegal Adulterants in Antihypertensive Functional Foods

Jielan Hu  1 , Li Zeng  1 , Ling He  2 , Fan You  2 , Chengjun Sun  3
Affiliations

Multiwalled Carbon Nanotubes-Dispersive Solid-Phase Extraction Coupled with UPLC-ESI-MS-MS for Simultaneous Determination of 10 Illegal Adulterants in Antihypertensive Functional Foods

Jielan Hu et al. J Chromatogr Sci. 2016 May-Jun.

Abstract

A reliable method for simultaneous determination of 10 illegal adulterants including chlortalidone, hydrochlorothiazide, indapamide, metoprolol, nifedipine, nimodipine, nitrendipine, reserpine, triamterene and valsartan in antihypertensive functional foods by ultra-high-performance liquid chromatography coupled with electrospray ionization-tandem mass spectrometry is presented in this article. The target chemicals were extracted with acetonitrile ultrasonically and cleaned up using multiwalled carbon nanotubes-dispersive solid-phase extraction. The separation was performed on a Waters ACQUITY UPLC BEH C18 Column (2.1 × 100 mm, 1.7 µm) with acetonitrile, 0.1% formic acid and 10 mmol/L ammonium acetate solution as mobile phase at a flow rate of 0.2 mL/min. Multiple reaction monitoring was applied for detection and sildenafil was used as the internal standard. The correlation coefficients of the method were >0.995, with the limits of detection of 0.022-0.30 ng/mL and the limits of quantification of 0.075-0.99 ng/mL. The interday and intraday relative standard deviations were <9.77% and the recoveries were in the range of 85.8-109%. The established method has been applied for the analysis of real samples, and reserpine was detected in a tonic wine sample with a content of 60.1 ± 3.2 mg/L.

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Figures

Figure 1.
Figure 1.
Q3 scan spectra of the 10 target chemicals (A–J) and the internal standard (K, L). This figure is available in black and white in print and in color at JCS online.
Figure 1.
Figure 1.
Q3 scan spectra of the 10 target chemicals (A–J) and the internal standard (K, L). This figure is available in black and white in print and in color at JCS online.
Figure 1.
Figure 1.
Q3 scan spectra of the 10 target chemicals (A–J) and the internal standard (K, L). This figure is available in black and white in print and in color at JCS online.
Figure 1.
Figure 1.
Q3 scan spectra of the 10 target chemicals (A–J) and the internal standard (K, L). This figure is available in black and white in print and in color at JCS online.
Figure 2.
Figure 2.
Under ESI+ mode, the total ion chromatogram and the mass spectrogram of the three chemicals and internal standard. Peak identification: 1-TAT, 2-MTR, 3-RSP and 4-sildenafil. This figure is available in black and white in print and in color at JCS online.
Figure 3.
Figure 3.
TIC and the mass spectrogram of seven target chemicals and the internal standard under ESI− mode. This figure is available in black and white in print and in color at JCS online.
Figure 4.
Figure 4.
The mass spectrogram of RSP detected in a tonic wine. This figure is available in black and white in print and in color at JCS online.
See this image and copyright information in PMC

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