summary
The method refers to the liquid chromatography tandem mass spectrometry (LC-MS/MS) detection method developed by the Chinese Pharmacopoeia in 2015, which is a method for identifying Chinese herbal medicines Ejiao, antler gum and tortoise shell gum. The method can fully meet the requirements of sensitivity and reproducibility of the identification method of the 2015 edition of Chinese Pharmacopoeia, Ejiao, Ejiao, Antler and Tortoise.
Principle of identification
Take 0.1 g of medicinal material powder, ultrasonically extract it with 1% ammonium bicarbonate solution, add excess trypsin to the continuous filtrate, and digest it at a constant temperature. The liquid-phase tandem mass spectrometer (LC-MS/MS) was used to detect the characteristic selection reaction monitoring ion pairs in the enzymatic hydrolysate. The signal-to-noise ratio of the peak should be greater than 3:1, and the chromatographic retention time of the reference drug is consistent. Chromatographic peak.
Sample preparation
Testing equipment
Tandem Mass Spectrometry System: Thermo ScientificTM TSQ Quantum Access MAXTM Triple Quadrupole Mass Spectrometer
High Performance Liquid Phase System: UltiMateTM 3000 Rapid Separation LC Systems Rapid Separation LC System
Detection instance
1. Typical chromatogram of medicinal gelatin, tortoise shell glue and antler gum
2. Comparison of typical chromatograms of medicinal Ejiao, Ejiao and Ejiao
It can be observed that in the figure below, the signal-to-noise ratio of the chromatographic peaks of Fig.4B medicinal Ejiao (purchased from Beijing Tongrentang) and Fig.4C medicinal Ejiao beads (purchased from Beijing Tongrentang) should be greater than 3:1, and presented simultaneously with Fig. 4A Ejiao reference drug chromatographic peak with consistent chromatographic retention time.
3. Comparison of typical chromatograms between suspected fake tortoise and suspicion of false antler gum and reference medicinal materials
It can be observed that in the chromatogram of Fig.5B suspected fake tortoise medicinal material (purchased from a certain medicinal materials market), there is no chromatographic peak consistent with the chromatographic retention time of the Fig. 5A tortoiseshell reference drug; similarly, Fig.6B In the chromatogram of the suspected false antler gum (purchased from a certain medicinal materials market), there is no chromatographic peak consistent with the chromatographic retention time of the Fig. 6A tortoiseshell reference drug.
3. Conclusion
In summary, the high performance liquid chromatography-mass spectrometer system consisting of the Thermo ScientificTM TSQ Quantum Access MAXTM triple quadrupole mass spectrometer and the UltiMateTM 3000 Rapid Separation LC Systems rapid separation liquid phase system can fully satisfy the Chinese Pharmacopoeia. The requirements of the identification method for the Chinese herbal medicine Ejiao, staghorn gum and tortoise shell glue in the 2 0 1 5 edition.
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