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Qualitative and quantitative method of triterpene saponins in traditional Chinese medicine by electrospray protonation fragmentation-mass spectrometry multiple reaction detection mode
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A technology for monitoring triterpenoid saponins and multiple reactions, which is applied in the field of chemical analysis and detection, and can solve the problems of low detection sensitivity and difficulty in quantification of traditional Chinese medicine saponins.
Active Publication Date: 2020-04-10
匡海学 +2
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While using electrospray tandem mass spectrometry in MRM mode, fragmentation of [M+Na] + and [M-H] - Precursor ions can achieve satisfactory quantitative results for the constant triterpene saponins in traditional Chinese medicine. However, the detection sensitivity of this method is low when detecting some traditional Chinese medicine saponins, and the quantification is difficult.
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Embodiment 1
[0037] Example 1 Establishment of a Quantitative Method for Triterpenoid Saponins from Paeoniae Ruba
[0038] 1 experimental equipment
[0039] Qtrap-4000 triple quadrupole linear ion trap mass spectrometer (AB SCIEX company, the United States); H-class ultra-high performance liquid chromatography (online degasser, automatic sampler, quaternary pump, American Waters company); ACQUITY UPLC HSS T3 chromatographic column (2.1×150mm, 1.8μm), connected to a Waters HSS T3 guard column (2.1×5mm, 1.8μm). Milli-Q water purifier (Millipore China Co., Ltd.), ML104 / 02 electronic analytical balance (Mettler Toledo Instruments Shanghai Co., Ltd.), Vortex 3000 vortex oscillator (Wiggens, Germany); Mikro 200R centrifugal Machine (Hettich, Germany), KQ-500DB CNC ultrasonic cleaner (Kunshan Ultrasonic Instrument Co., Ltd.).
[0040] 2 Preparation of standard products
[0041] Accurately weigh 1-9 kinds of saponin standard items ( figure 1 Shown) appropriate amount, accurately weighed, add m...
Embodiment 2
[0063] Example 2 Establishment of Liaodong Aralia triterpene saponin quantitative method
[0064] 1. Experimental equipment
[0065] With embodiment 1.
[0066] 2. Preparation of standard products
[0067] Accurately weigh 1-10 saponin standard items ( image 3 Shown) appropriate amount, accurately weighed, add methanol and be mixed with the mixed reference solution that mass concentration is respectively 1.69, 0.21, 0.20, 0.28, 1.00, 0.98, 1.04, 1.00, 1.00, 1.00mg / ml as stock solution, in 4 Store at ℃ for later use.
[0068] 3. Optimizing DP, CE and CXP mass spectrometry parameters based on response surface center composition design
[0070] Using mass spectrometry in multiple reaction monitoring (MRM) mode, using saponins 1-10 as template compounds, the response value and reproducibility of proton / ammonium ion cleavage targeted ion pairs were optimized by response surface methodology. According to th...
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technical field [0001] The invention relates to a method for quantifying triterpene saponins in traditional Chinese medicine, in particular to a method for qualitatively and quantitatively determining triterpene saponins in traditional Chinese medicine based on electrosprayprotonationcracking-mass spectrometry multiple reaction detection mode. The invention belongs to the technical field of chemical analysis and detection. Background technique [0002] Triterpene saponins have been widely accepted by researchers as the main effective parts or groups of effective parts in traditional Chinese medicine. However, triterpene saponin molecules lack chromophores, absorb ultraviolet light at the end, and are non-volatile. Therefore, there is currently a lack of effective methods for the quantification of triterpene saponins. At present, the quantitative methods of triterpene saponins in traditional Chinese medicine mainly use high performance liquid chromatography-ultraviolet spe...
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