Objective: To establish a GC-MS characteristic chromatogram of Huatuo Jiuxin pills and to develop simultaneous determination method of borneol, isborneol and muscone in the sample. Methods: GC-MS analysis was performed on a VF-WAXms column (0.25 mm×30 m,0.25 μm). The column temperature was programmed to start at 140 ℃ maintaining for 2 min, and rose to 230 ℃ at a rate of 35 ℃·min-1, maintaining for 5 min. The inlet temperature was 210 ℃ and the detector temperature was 250 ℃. The ion source was electrospray ion source, with the ion source of 300 ℃, MS quadrupole temperature of 150 ℃, the emission current of 34.6 μA, the ionization energy of 70 eV and the solvent delay of 3 min, quantized by the full scan method.Traditional Chinese medicine chromatographic fingerprint similarity evaluation software(2012 version)was used for similarity analysis in 12 batches of Huatuo Jiuxin pills, and the contents of borneol, isoborneol and muscone in 12 batches of samples were determined at the same time. Results: The GC-MS characteristic chromatogram of Huatuo Jiuxin pills was established, and the similarities between the characteristic chromatogram and chromatograms of 12 batches of Huatuo Jiuxin pills were above 0.999. There were altogether 8 common peaks, and 3 of them were identified as isoborneol,borneol andmuscone, respectively. The contents of borneol, isborneol and muscone in 12 batches of samples were in the range of 0.875 7-1.525 0, 0.730 4-1.140 5, 0.097 1-0.112 0 g per pill, respectively. Conclusion: The combination of the GC-MS characteristic chromatogram and content determination of three components can reflect inherent quality of volatile chemical components in Huatuo Jiuxin pills. The method is simple, feasible, accurate, stable, repeatable and specific, and can provide a reference for the quality control of Huatuo Jiuxin pills.
CHEN Fang-yuan, ZHANG Yun-jing, ZHAO Bing, LI Long-fei, LI Ping-ping, PENG Can, WU De-ling, XIE Zi-li, WU Hong
. GC-MS characteristic chromatogram and assay of three components for Huatuo Jiuxin pills*[J]. Chinese Journal of Pharmaceutical Analysis, 2022
, 42(11)
: 1917
-1926
.
DOI: 10.16155/j.0254-1793.2022.11.07
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