Determination of the content of cinnamic aldehyde in Dubadazhitong Babu by gas chromatography

Abstract: Aldehydes can be divided into fatty aldehydes, ester aldehydes, aromatic aldehydes and terpene aldehydes. Fatty aldehyde refers to a type of aldehyde in which carbon atoms in a molecule are connected in a chain, and is in an open chain. Alicyclic aldehyde refers to the carbon atoms in the molecule connected to form a closed carbon ring. The carbonyl group of the aromatic aldehyde is directly connected to the aromatic ring. Terpene aldehyde is a branch of terpenoids.

Objective To establish a gas chromatographic method for simultaneous determination of the contents of camphor, menthol, methyl salicylate, cinnamaldehyde, and eugenol in Paida Zhitong Babu. Methods The volatile oil component in the sample was extracted by the volatile oil extraction method to prepare a sample solution. A quartz capillary column (phenomenexZB-WAX, length 30m, inner diameter 0.32mm, coating 0.5μm) was used as the chromatographic column, nitrogen was used as the carrier gas, and FID detector , Using temperature programming, internal standard method to determine the content of 5 components in the sample. Results Camphor, menthol, methyl salicylate, cinnamaldehyde, and eugenol were well separated under the same chromatographic conditions, and the linear relationship was good. The average sample recovery rates (n = 6) were 98.32%, 97.43%, and 95.89%, respectively. , 96.26%, 98.78%. Conclusion This method is simple and accurate, and can be used for the quality control of analgesic babu.

[Keywords] camphor; menthol; methyl salicylate; cinnamaldehyde; eugenol; capillary gas chromatography

Painkiller analgesic cataplasm is a hydrogel plaster made from 77 kinds of Chinese medicines such as hematoxylin, peach, safflower, etc. after supercritical carbon dioxide extraction, and added with 9 kinds of volatile oils such as cinnamon oil, clove basil oil, etc. The effects of reducing blood stasis, reducing swelling and hemostasis, qi and analgesia, and converging muscles have a significant effect on the treatment of bruises, burns, burns, and stab wounds [1]. The babu is a new type of plaster preparation made by mixing Chinese herbal medicine extracts with a hydrophilic matrix and coating on a backing material. The volatile oil part mainly contains methyl salicylate, cassia oil, clove basil oil, etc. The main component of cinnamon oil is cinnamaldehyde, and the main component of clove basil oil is eugenol. In this paper, according to the characteristics of its dosage form, capillary gas chromatography is used to simultaneously determine the contents of 5 main components [2, 3].

1 Instruments and reagents

American Agilent 6890N gas chromatograph and supporting workstation, quartz capillary column (phenomenex company); camphor reference substance (lot number 747-200606), menthol reference substance (lot number 0728-00005), methyl salicylate reference substance (lot number 110707-200107 ), Cinnamic aldehyde reference substance (lot number 110710-200714), eugenol reference substance (lot number 725-200209), the above reference substances were purchased from China National Institute for the Control of Pharmaceutical and Biological Products, naphthalene (purity> 99%, sigma); Babu agent (provided by Guangzhou Jingxiutang Pharmaceutical Factory, batch number: 081109, 081116, 081117, 081118, 081119, 081120, specifications: 10cm × 6cm); nitrogen, hydrogen and air are high-purity gases, other reagents are analytically pure , Water is pure water.

2 Methods and results

2.1 Preparation of mixed reference substance solution Weigh the appropriate amount of camphor, menthol, methyl salicylate, cinnamaldehyde, eugenol reference substance, add absolute ethanol to make a solution containing 1mg per ml, shake well, that is, you get.

2.2 Preparation of internal standard solution Precisely weigh an appropriate amount of naphthalene, add absolute ethanol to make a solution containing 10mg per milliliter, shake well, and get.

2.3 Preparation of test solution Take 5 tablets of Paida Pain Relief (with ointment 30g), cut into 1cm wide strips, remove the cap liner, place in a 1000ml round bottom flask, add 500ml of water, connect the volatile oil extractor, from Add water to the top of the extractor to fill the scale and overflow into the flask. Connect the reflux condenser tube, heat and reflux for 5h, let cool, separate the oil layer, filter with a funnel covered with anhydrous sodium sulfate, and weigh the weight accurately. Accurately weigh 100μg of volatile oil, add 250μl of internal standard solution, dilute to 10ml with absolute ethanol, shake well, and you get it.

2.4 Preparation of negative control solution Take negative samples of eucalyptus oil, camphor, peppermint oil, borneol, methyl salicylate, star anise oil, cassia oil, and clove basil oil, and process the solution in the same way as the test solution.

2.5 Chromatographic conditions Chromatographic column: ZB-WAX capillary column (30m × 0.32mm, 0.5μm), fixed liquid is polyethylene glycol (PolyethyleneGlycol); carrier gas: N2, column flow rate: 1.0ml · min-1; inlet The temperature is 210 ℃, the injection volume is 1μl, the split injection, the split ratio is 40: 1; the detector is a hydrogen flame ionization detector (FID), the temperature is 245 ℃; the column temperature is programmed to increase the temperature, and the temperature is kept at 80 ℃ for 2min The temperature was started, and the temperature was raised to 140 ° C at 5 ° C / min for 8 minutes, and then increased to 220 ° C at 12 ° C / min for 2 minutes.

2.6 System adaptability Precisely measure the appropriate amount of the mixed reference solution and the naphthalene internal standard solution, dilute with absolute ethanol to 10ml, and draw 1μl for injection measurement. The retention time of the five peaks is within 30min, and the peak resolution of each index is uniform. If it is greater than 1.5, the number of theoretical plates is not less than 6000, which meets the requirements of pharmacopoeia content determination. The chromatogram is shown in Figure 1 ~ 4. Figure 1 Chromatogram of test solution Figure 2 Chromatogram of mixed reference solution Figure 3 Chromatogram of internal standard solution Figure 4 Chromatogram of negative control solution

2.7 Methodological survey

2.7.1 Investigation of linear relationship Precisely draw 0.5, 1.5, 2.5, 3.5, 5.0 ml of mixed reference solution, add 250 μl of internal standard solution precisely, dilute to 10 ml with absolute ethanol, shake well, and pass 0.22 μm microporous membrane After filtration, 1 μl was injected to determine the peak area. The ratio of the peak area of ​​each index to the peak area of ​​the internal standard is taken as the ordinate (Y), and the ratio of the concentration of each reference substance and the concentration of the internal standard is taken as the abscissa (X) for linear regression. Camphor, menthol, and salicylic acid are obtained. The regression equations for methyl ester, cinnamaldehyde and eugenol are: Y = 0.63207X 0.15990, r = 0.99968.Y = 0.56908X 0.04303, r = 0.99936.Y = 0.88323X 0.05737, r = 0.99951.Y = 0.61575X 0.03480, r = 0.99945.Y = 0.57945X 0.04344, r = 0.99985. The linear range is 56.0 ~ 560μg · ml-1, 60.5 ~ 605μg · ml-1, 57.0 ~ 570.0μg · ml-1, 58.5 ~ 585.0μg · ml- 1,59.5 ~ 595.0μg · ml-1.

2.7.2 Precision experiment The same test solution was accurately pipetted and continuously measured for 5 times. The average peak area ratio RSD of camphor, menthol, methyl salicylate, cinnamaldehyde, eugenol and internal standard were respectively 0.63%, 0.76%, 1.17%, 0.85%, 0.95%.

2.7.3 Repeatable experiment: Take 7 parts of Paida Pain Relief (Batch No .: 081109), 5 tablets each, make the test solution according to the method under "2.3", and determine according to the law. Results The average peak area ratios RSD of camphor, menthol, methyl salicylate, cinnamaldehyde, eugenol and internal standard were 1.80%, 1.16%, 2.19%, 1.09%, 1.45%, respectively.

2.7.4 Stability laboratory temperature and dark conditions, the same test solution was taken at 0, 2, 4, 6, 8, 24h injection 1μl to determine the peak area, the results camphor, menthol, methyl salicylate , The average peak area ratio RSD of cinnamaldehyde, eugenol and internal standard were 1.61%, 0.93%, 1.10%, 1.97%, 1.67%, respectively.

2.7.5 Sample recovery rate Take 6 copies of the finished product of beat analgesic cataplasm with a known content (lot number: 081109), 3 pieces each, cut into 1cm wide strips, remove the cap liner, and place in a 1000ml round bottom flask. Accurately add camphor, menthol, methyl salicylate, cinnamaldehyde, eugenol reference substance solution, prepare the test article solution according to the method under "2.3", filter through 0.22μm microporous membrane and inject 1μl to measure the peak Area, calculate the recovery rate of the sample. The results are shown in Table 1. Table 1 Experimental results of sample recovery rate

2.7.6 Determination of sample content Take 5 batches of finished cataplasms, prepare the test solution according to the above method, accurately draw 1μl into the gas chromatograph to determine the peak area, and calculate the eugenol content according to the internal standard method. The results are shown in Table 2. Table 2 Sample content determination results

3 Discussion

The preparation of the test solution used methanol leaching method. The obtained test solution is not only large in volume, but also has many impurity components. The glycerin in the matrix of the cloth is also proposed, which affects the life of the gas chromatography column. The volatile oil extraction method is used to prepare the test product solution, and the operation repeatability is good. The extraction rate of each component within 5 hours can also be close to 100%, and the content determination impurities do not interfere, which can effectively control the quality of the preparation. In the study, I tried to use n-hexadecane and cyclohexanone as internal standards, but it was not used because of the chromatographic peak separation effect and inappropriate retention time. This study not only measured the content of multiple volatile components in the Paida Pain Relief Papules under the same gas chromatographic conditions, but also provided a methodological reference for the control of the content of the volatile components of the topical plaster type.

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