The content was determined by the newly opened reference substance, and the cinnamaldehyde reference substance was unstable. The reference solution should be freshly prepared.
Objective To establish a method for the determination of cinnamaldehyde in cinnamon oil and to identify volatile chemical constituents. Method: Gas chromatography , cinnamon oil is Cinnamomum cassia Presl dry branch, leaf steam distillation to obtain volatile oil. 3mm4m stainless steel column, 10% PEG-20M as fixative, ChromosorbWAW6080 mesh support, FID detector, column temperature 190 °C; GC/MS, with HP-5 capillary column, column temperature starting at 120 ° C for 5 min, 5 ° C.min-1 heating to 150 ° C for 7 min to detect the mass-to-charge ratio range 10425. Results: Cinnamaldehyde at 210 mg.mL-1 There is a good linear relationship in the range, and the average recovery rate is 98.3% 101.6% RSD ≤ 1.3%. The gasification and mass spectrometry identified 39 compounds. Conclusion: The method is simple, rapid and accurate, and can effectively exclude the interference of other components.
The main component is cinnamaldehyde (Cinnamicaldehyd current quality standard Chinese Pharmacopoeia (1995 edition) uses an excessive amount of sodium bisulfite, cinnamaldehyde and sodium bisulfite form a red precipitate, the precipitate is dissolved in the water layer and separated from the oil layer, read Calculating the volume of the oil layer, the method is simple, but the cycle is long, the error is large, and when the sample is mixed with other aldehydes, the result measured by the method is high. The content of the method is determined by gas chromatography, and the method is simple and rapid. It can eliminate the interference of other impurities. This paper also applies the GC-MS to identify the volatile components in cinnamon oil.
1 instruments and reagents
Origin Guangxi) Japan ShimadzuGC-17A; C-R6A data processor; US HP5890 gas chromatograph; HP-MS detector; NBS75K. Anhydrous ethanol (AR cinnamaldehyde reference product (provided by China National Institute for the Control of Pharmaceutical and Biological Products) Cinnamon oil (commercially available. Gas chromatograph)
2 solution preparation
Dilute to the mark with absolute ethanol. 2.1 Preparation of the reference solution The cinnamic aldehyde reference substance was accurately weighed into a 25 mL volumetric flask.
Dilute to the mark with absolute ethanol, 2.2 Preparation of the sample solution accurately weighed the sample about 0.05g into a 10mL volumetric flask. Shake well as a test solution.
3 experimental conditions and their investigation
3.1 chromatographic conditions
10% PEG-20M fixative, 3.1.1 packed column gas chromatography column conditions 4mm3m stainless steel column. ChromosorbWAW6080 mesh carrier, FID detector, column temperature 190 ° C, detector temperature 230 ° C, carrier gas: nitrogen 60 mL.min-1 hydrogen, air pressure: 50kPa
Split ratio 40:1 flow rate 1.0mL.min-1 Column temperature: start at 120 ° C for 5 min, then heat up to 150 ° C at 5 ° C.min-1 for 7 min to detect the mass-to-charge ratio range 10425 ion source temperature 300 ° C, 3.1.2 GC/MS system conditions HP-55% benzene substituted methyl silicone) capillary column (0.25mm30m carrier gas: helium gas. Multiplication voltage 1500eV
Diluted with absolute ethanol to the scale as a reference stock solution, 3.2 linear relationship was investigated to accurately weigh the cinnamic aldehyde reference substance 0.5g into a 25mL volumetric flask. Accurately measure 12345mL in a 10mL volumetric flask, dilute to the mark with absolute ethanol, and inject 3μL into the gas chromatograph, record the chromatogram, take the sample concentration as the abscissa, the peak area as the ordinate, and make the regression curve and regression equation. n=3 is:
Y=3.0104X-5.3102r=0.9999
Cinnamaldehyde has a good linear relationship in the range of 210 mg.mL-1.
The peak area RSD was 1.29% indicating that the sample was stable within 10 h. 3.3 Stability test The precision sample solution was injected at 0124610h.
According to the sample determination method, it was determined 8 times according to law, and the 3.4 reproducibility test took the same batch of samples. The average content was 79.7% and the RSD was 0.88%.
Approximately 0.03 g of each of the 0.03 g precision-added cinnamic aldehyde reference materials in each 10 mL volumetric flask was used. The 3.5 sample recovery rate test accurately weighed 6 parts of the same batch of cinnamon oil sample with the determined content. Dilute to the mark with absolute ethanol, shake well, and inject 3 μL into the gas chromatograph, record the measurement chromatogram, and measure each sample 3 times. The recovery rate of the sample is 98.3%, 101.6%, and the large RSD is 1.3%.
Record the chromatographic results, 3.6 sample determination results, respectively, draw the reference solution and 3 μL of the test solution into the gas chromatograph. Calculated; another 10mL of the same batch of samples was determined according to the Chinese Pharmacopoeia 1995 edition method.
41 components were separated from cinnamon oil, and 3.7 GC/MS analysis was used to take 0.2 μL of essential oil and directly injected according to the conditions of GC/MS. Under the above conditions. 39 ingredients were identified, accounting for 95.1% of all essential oils
4 results and discussion
All aldehydes, methyl ketones and cyclic ketones reacted with sodium hydrogen sulfite. From the results of gas chromatography analysis, it was found that cinnamyl alcohol, vanillin and 2-methoxycinnamaldehyde were contained in cinnamon oil. The results of the determination of the pharmacopoeia method are high.
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