Method for detecting Smilax smilax fumigated by sulfur and its products
A technology of sulfur fumigation and Smilax smilax, which is applied in the field of detection of sulfur fumigated Smilax smilax and its products, can solve the problems that the rapid detection method of sulfur fumigation Smilax smilax has not been reported yet, and achieves accurate and reliable calculation results, good effect, and economical the effect of time
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Embodiment 1
[0037] Step 1. Take the fresh Smilax smilax medicinal material and the sulfur-fumigated Smilax smilax medicinal material, slice and dry them separately, and then grind them into powders. Take 0.5g of each and place them in 50ml volumetric flasks, add 20mL of 80% methanol, and use ultrasonic extraction to extract 20- Take it out after 30 minutes, cool to room temperature, add 80% methanol to the volume, shake well, filter, and take the subsequent filtrate as sample solution a and sample solution b.
[0038]Step 2, using ultra-high performance liquid chromatography-quadrupole-time-of-flight mass spectrometry to collect ion fragment mass spectrometry data for sample solution a and sample solution b respectively, wherein the chromatographic conditions are: use ACQUITY UPLC HSS T3 chromatographic column ( 2.1mm×100mm, 1.8μm); Gradient elution is adopted, phase A in the mobile phase is 0.1% formic acid aqueous solution, phase B is acetonitrile, and the ratio of acetonitrile is: 5–10%...
Embodiment 2
[0050] On the basis of Example 1, the following steps are added after step 1 and before step 2: add 1.0×10 -4 mol / L catechol PBS buffer solution, the pH value of the selected PBS buffer solution is 7.4, the phosphate concentration is 0.1mol / L, and a three-electrode system with a glassy carbon electrode as the working electrode is used to add The sample solution a and sample solution b with PBS buffer solution were scanned by cyclic voltammetry, and the scanning parameters were set as: initial potential -0.4V, highest potential 1V, lowest point -0.4V, final potential -0.4V, scan rate 0.05V / s, scan times 2 times, sensitivity 10 -4 A / V, waiting time is 2s.
[0051] After the above steps, the time required for ultra-high performance liquid chromatography-quadrupole-time-of-flight mass spectrometry is further shortened. At the same time, after the heavy metal ions in the sample solution are quickly separated, some invalid mass spectra that affect the analysis are also eliminated. ...
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