- 中文核心期刊
- CA、AA收录期刊
- 中国机械工程学会理化检验分会会刊
| Citation: |
YAN Chuanyong, ZHENG Jia, MA Luyao, XI Cunxian, GUO Siyan, ZHANG Wenhua, MU Zhaode. Establishment of Mass Spectrometry Database for 97 Chemical Drugs and Qualitative Analysis of Chemical Drugs in Health Products by Ultra-High Performance Liquid Chromatography-Quadrupole/Electrostatic Field Orbitrap High Resolution Mass Spectrometry[J]. PHYSICAL TESTING AND CHEMICAL ANALYSIS PART B:CHEMICAL ANALYSIS, 2024, 60(11): 1173-1182. DOI: 10.11973/lhjy-hx230407
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2.00 g of the sample was taken, and placed in a 50 mL-stoppered centrifuge tube. 10 mL of extraction agent was added [extraction agent for tablet, capsule, powder, and oral liquid samples was acetonitrile, extraction agent for health wine samples was a mixture of acetonitrile-water-formic acid at a volume ratio of 60∶39∶1, and extraction agent for soft gel and health tea samples was 60% (volume fraction) methanol solution]. The mixture was vortex mixed, shaken for 30 min and centrifuged at a rotational speed of 3 500 r·min−1 for 3 min at 4 ℃. The supernatant was taken, and blown to near dryness by nitrogen at 40 ℃. 1 mL of extraction agent was added, and the mixture was vortex dissolved for 30 s. The solution was passed through a 0.22 μm nylon filter membrane, and the 97 chemical drugs in the filtrate was analyzed by ultra-high performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry (UHPLC-Q-Orbitrap HRMS). Hypersil GOLD chromatographic column was used as the stationary phase and the mixed solution composed of methanol solution containing 0.1% (volume fraction) formic acid and 2.0 mmol·L−1 ammonium acetate solution at different volume ratios was used as the mobile phase for gradient elution. Heating electrospray ion (HESI) source was used for mass spectrometry. The resolution was set to 70 000 and the ion implantation time (IT) was 100 ms in primary mass spectrometry full scan (Full MS) mode, while the resolution was set to 17 500 and the IT was 50 ms in the data dependent secondary mass spectrometry scanning (dd-MS2) mode. As shown by the results, the detection limits of 97 chemical drugs in solid matrix (tablet, capsule, and powder), oral liquid, health wine, health tea and soft gel were in the ranges of 1.22-68.20 μg·kg−1, 2.25-101.41 μg·kg−1, 1.38-39.80 μg·kg−1, 2.70-93.52 μg·kg−1, and 2.50-71.76 μg·kg−1, respectively. This method was used for the analysis of 50 samples of health product, and nandrolone phenylpropionate, medroxyprogesterone acetate, acetaminophen, and mevastatin in 5 samples were detected.
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