CN112034071A - Fingerprint spectrum detection method of medicinal sesame oil - Google Patents
Fingerprint spectrum detection method of medicinal sesame oil Download PDFInfo
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Abstract
The invention relates to a fingerprint detection method of medicinal sesame oil, which comprises the steps of taking at least one of methyl palmitate, methyl stearate, methyl elactoate, methyl oleate, methyl linoleate, methyl arachidate, cis-11-eicosenoic acid methyl ester, methyl linolenate, methyl behenate and methyl lignocamate as an effective component, and carrying out at least one of gas chromatography content determination and gas chromatography fingerprint construction by using the effective component. The invention researches the fingerprint of the medicinal sesame oil, establishes the determination condition of the gas chromatography fingerprint, performs methodology investigation, prepares the standard of the gas chromatography fingerprint of the medicinal sesame oil according to a plurality of batches of large-scale production samples, can effectively standardize production operation in the production process, ensures the stable quality of the final products of the medicinal sesame oil and also ensures the control quality of the downstream products.
Description
Technical Field
The invention belongs to the field of detection of pharmaceutic adjuvants, and particularly relates to a fingerprint spectrum detection method of medicinal sesame oil.
Background
The sesame oil processed and prepared by the traditional water substitution method in China has unique flavor and is a favorite condiment and a good cooking accessory. Although the sesame oil contains more than 80% of unsaturated fatty acids such as oleic acid (O), linoleic acid (L) and the like, the sesame oil has good stability and long shelf life due to the rich natural vitamin E and various types of lignans such as sesamin, sesamolin, sesamol and the like. Because of the low yield of the sesame oil and the rich nutrition and market value, the market price of the sesame oil is far higher than that of common bulk oil varieties such as soybean oil, rapeseed oil, peanut oil, cottonseed oil and the like. In order to obtain higher profit, part of illegal producers add other cheap vegetable oil into the sesame oil, and even add inedible oil such as tung oil, mineral oil, castor oil, etc., or directly mix essence and spice with other low-price vegetable oil to be sold as sesame oil. Adulterated sesame oil not only has serious quality problem, but also brings harm to physical and mental health of consumers, and seriously damages the benefits of the consumers and legal operators. In order to effectively inhibit the behaviors, a scientific, rapid, accurate and effective detection method needs to be established for identifying adulteration of the sesame oil.
The adulteration detection of the sesame oil which is obtained by blending the sesame oil with the non-edible oil and the cheap vegetable oil with the essence can be distinguished according to the special properties of the non-edible oil or the color development property of lignin substances in the sesame oil. For sesame oil blended with inexpensive vegetable oils, different kinds of oils have different inherent characteristics such as color, smell, taste, characteristic components, triglyceride structure and fatty acid composition. The purity of sesame oil can be judged by identifying whether these vegetable oils are present in sesame oil, and for example, specific components such as erucic acid in rapeseed oil, gossypol in cottonseed oil, and long-chain fatty acids having twenty carbons or more in peanut oil are used as the basis for judging the presence of these oils. With the improvement of breeding and processing technology, characteristic components gradually can not be used as a basis for identifying the types of the grease. And some methods are not always effective due to the similarity of physicochemical characteristics between vegetable oils. For example, the sensory test method is simple and easy to implement, is suitable for the detection of certain vegetable oils to a certain extent, has certain requirements on sensitive judgment capability and practical experience of testers, and can only be used as preliminary judgment on whether adulteration occurs or not.
At present, the detection method for doping cheap edible vegetable oil into sesame oil can be mainly divided into two types, and firstly, the sesame oil is identified according to the characteristic component properties of the sesame oil; and secondly, identifying according to the properties of the grease. The detection method based on the characteristic substances in the sesame oil comprises the following steps: ultraviolet spectrophotometry: the lignan substance in the sesame oil has characteristic absorption in an ultraviolet region, and is qualitatively and quantitatively detected by an ultraviolet spectrophotometry; ② a color development method: the specific reaction between the characteristic components in the sesame oil, such as sesamol, sesamin and other lignan compounds, and a color developing agent is utilized to generate a compound with a certain color, and the color depth of the compound is related to the content of the sesame oil, so that the purity of the sesame oil in an oil sample is judged; ③ high performance liquid chromatography: mainly utilizing high performance liquid chromatography to measure the contents of sesamin and sesamolin in the sesame oil; fourthly, electronic nose method: the authenticity is judged mainly by analyzing the rich fragrance components in the sesame oil; fluorescent spectrometry: the edible vegetable oil adulteration detection method is based on aromatic ring structures with different functional groups in different vegetable oil structures and fluorescent components such as unsaturated fatty acid and the like. Secondly, the method for detecting the composition and the content of the triglyceride and the fatty acid in the vegetable oil comprises the following steps: gas chromatography: because the triglyceride structure and the composition and the content of fatty acid in different vegetable oil are different, the composition and the content of main fatty acid oleic acid and linoleic acid of sesame oil are influenced certainly after the sesame oil is adulterated, the composition and the content of the fatty acid are analyzed by gas chromatography, and the adulterated sesame oil can be identified by comparing the composition and the content with corresponding pure oil; ② high performance liquid chromatography: the content of triglyceride and fatty acid in the sesame oil is mainly determined by high performance liquid chromatography; ③ the combined use method: the method adopts gas-liquid phase combined method, gas-mass spectrum combined method and liquid-mass spectrum combined method; fourthly, infrared spectroscopy: the infrared absorption spectrum can reflect the molecular structure information of different oils and fats, and the oils and fats can be expressed essentially.
The fingerprint refers to a spectrogram or an image of a chromatogram or a spectrum which can mark the characteristics of a sample obtained by properly processing the sample and adopting a certain analysis means such as the spectrum or the chromatogram. These maps or images are unique and representative, just like a human fingerprint, and are therefore visually referred to as fingerprints. The fingerprint spectrum can be used for determining various chemical components of the sample without quantification, provides the outflow curve characteristics of the grease components, can also find out the related trace components of the sesame oil and the regular characteristics of the quantity ratio relationship thereof, and can effectively embody the integrity and the comprehensive action of the product, so the fingerprint spectrum technology can be applied to the analysis and the quality identification of the grease, and provides a reference basis for identifying counterfeit and inferior sesame oil. At present, the fingerprint spectrum technology has certain research in the aspects of analysis of traditional Chinese medicines, tobacco and wines. In contrast, the traditional Chinese medicine fingerprint spectrum technology is mature, but the methods are similar in the spectrogram analysis process, so that the information in the spectrum is sufficiently explored by referring to each other, and the grease fingerprint spectrum is more scientifically established.
Disclosure of Invention
In view of the above, the invention aims to provide a method for detecting the fingerprint of the medicinal sesame oil, so that the medicinal sesame oil fingerprint is researched, the gas chromatography fingerprint measurement condition is established, methodology investigation is carried out, the gas chromatography fingerprint standard of the medicinal sesame oil is formulated according to a plurality of batches of large-scale production samples, the production operation can be effectively standardized in the production process, the stable quality of the medicinal sesame oil final product is ensured, and the quality control of the downstream product is also ensured.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
a fingerprint detection method for medicinal oleum Sesami comprises taking at least one of methyl palmitate, methyl stearate, methyl elaeate, methyl oleate, methyl linoleate, methyl arachidate, cis-11-eicosenoic acid methyl ester, methyl linolenate, methyl behenate and methyl lignocerate as effective component, and performing at least one of gas chromatography content determination and gas chromatography fingerprint construction with the effective component.
Further, the gas chromatography conditions were: using a strong polarity capillary chromatography column; carrier gas: nitrogen with flow rate of 0.5-2.0 ml/min; vaporization chamber temperature: 300 ℃ to 330 ℃; the sample amount is 0.1-0.5 mul; tail blowing: 40-60 ml/min; split-flow sampling with split-flow ratio (50-70) 1; a detector: a hydrogen flame ionization detector with the temperature of 250-280 ℃; the hydrogen flow rate is 30-50ml/min, and the air flow rate is 300-500 ml/min; temperature programming: the initial temperature is 90-110 ℃, the temperature is kept constant for 10-15min, the temperature is increased to 180 ℃ at 10 ℃/min, the temperature is kept constant for 5-10min, the temperature is increased to 200 ℃ at 0.5 ℃/min, the temperature is kept constant for 5-10min, the temperature is increased to 230 ℃ at 1 ℃/min, and the temperature is kept constant for 8-12 min.
Further, the gas chromatography conditions were: using a strong polarity capillary chromatography column; carrier gas: nitrogen gas; flow rate: 1 ml/min; a detector: detector Temperature (TD)280 ℃; a hydrogen Flame Ionization Detector (FID); the hydrogen flow rate was 30ml/min and the air flow rate was 400 ml/min. Sample inlet temperature: 320 ℃; the sample amount is 1 mul; tail blowing: 30 ml/min; a hydrogen Flame Ionization Detector (FID); the split ratio is 60: 1; temperature programming: the initial temperature is 100 ℃, the temperature is kept for 13min, the temperature is increased to 180 ℃ at the speed of 10 ℃/min, the temperature is kept for 6min, the temperature is increased to 200 ℃ at the speed of 0.5 ℃/min, the temperature is kept for 5min, the temperature is increased to 230 ℃ at the speed of 1 ℃/min, and the temperature is kept for 10.5 min.
Further, the relative retention time of methyl palmitate to methyl stearate is 0.84-0.86, the relative retention time of methyl palmitate to methyl stearate is 0.88-0.91, the relative retention time of methyl elactoate to methyl stearate is 1.03-1.05, the relative retention time of methyl oleate to methyl stearate is 1.05-1.07, the relative retention time of methyl linoleate to methyl stearate is 1.15-1.17, the relative retention time of methyl arachidate to methyl stearate is 1.18-1.20, the relative retention time of cis-11-eicosanoate to methyl stearate is 1.25-1.27, the relative retention time of methyl linolenate to methyl stearate is 1.27-1.29, the relative retention time of methyl behenate to methyl stearate is 1.43-1.45, and the relative retention time of methyl lignocerate to methyl stearate is 1.73-1.75.
Further, the relative retention time of methyl palmitate to methyl stearate was 0.85, the relative retention time of methyl palmitate to methyl stearate was 0.90, the relative retention time of methyl elactoate to methyl stearate was 1.04, the relative retention time of methyl oleate to methyl stearate was 1.06, the relative retention time of methyl linoleate to methyl stearate was 1.16, the relative retention time of methyl arachidate to methyl stearate was 1.19, the relative retention time of methyl cis-11-eicosenoate to methyl stearate was 1.26, the relative retention time of methyl linolenate to methyl stearate was 1.28, the relative retention time of methyl behenate to methyl stearate was 1.44, and the relative retention time of methyl lignocerate to methyl stearate was 1.74.
Further, the relative peak area of methyl palmitate relative to methyl stearate is 1.7-1.8, the relative peak area of methyl palmitate relative to methyl stearate is 0.01-0.03, the relative peak area of methyl elactoate relative to methyl stearate is 0.03-0.06, the relative peak area of methyl oleate relative to methyl stearate is 7.1-7.4, the relative peak area of methyl linoleate relative to methyl stearate is 9.00-9.20, the relative peak area of methyl arachidate relative to methyl stearate is 0.10-0.20, the relative peak area of cis-11-eicosenoic acid methyl ester relative to methyl stearate is 0.02-0.06, the relative peak area of methyl linolenate relative to methyl stearate is 0.04-0.08, the relative peak area of methyl behenate relative to methyl stearate is 0.01-0.05, and the relative peak area of methyl lignocerate relative to methyl stearate is 0.01-0.04.
Further, the relative peak area of methyl palmitate with respect to methyl stearate was 1.75, the relative peak area of methyl palmitate with respect to methyl stearate was 0.02, the relative peak area of methyl elactoate with respect to methyl stearate was 0.05, the relative peak area of methyl oleate with respect to methyl stearate was 7.27, the relative peak area of methyl linoleate with respect to methyl stearate was 9.07, the relative peak area of methyl arachidate with respect to methyl stearate was 0.11, the relative peak area of cis-11-eicosapentaenoate with respect to methyl stearate was 0.04, the relative peak area of methyl linolenate with respect to methyl stearate was 0.06, the relative peak area of methyl behenate with respect to methyl stearate was 0.03, and the relative peak area of methyl lignocamate with respect to methyl stearate was 0.02.
The invention has the beneficial effects that:
the invention researches the fingerprint of the medicinal sesame oil, establishes the determination condition of the gas chromatography fingerprint, performs methodology investigation, prepares the standard of the gas chromatography fingerprint of the medicinal sesame oil according to a plurality of batches of large-scale production samples, can effectively standardize production operation in the production process, ensures the stable quality of the final products of the medicinal sesame oil and also ensures the control quality of the downstream products. In addition, the identification of the measured fingerprint adopts a traditional Chinese medicine chromatogram fingerprint similarity evaluation system provided by the State pharmacopoeia Committee, the operation is convenient and fast, the similarity result is obtained, the fingerprint of the medicinal sesame oil product is evaluated, and the conclusion is objective and accurate.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and, together with the description, serve to explain the invention without limitation. In the drawings:
FIG. 1 shows finger prints of 10 batches of medicinal sesame oil; wherein, S1-S10 correspond to 10 batches of medicinal sesame oil samples respectively;
FIG. 2 shows standard finger prints of medicinal sesame oil.
Detailed Description
It should be noted that the embodiments and features of the embodiments of the present invention may be combined with each other without conflict.
The invention will be described in detail with reference to the following embodiments with reference to the attached drawings.
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict. The raw materials used in the invention are all commercial products, and the specific implementation process is as follows:
1. name (R)
Name: medicinal oleum Sesami.
2. The source of the test sample is as follows: tianjin Da Rentang Jingwanhong pharmaceutical Co., Ltd.
3. Preparation of test solution
Weighing 0.2g of medicinal sesame oil sample, filling the medicinal sesame oil sample into a 10ml test tube with a plug, adding 2ml of n-heptane for dissolving, then adding 2ml of 0.4mol/L potassium hydroxide solution, carrying out ultrasonic treatment for 10min until the solution is clear and has no oil drops, adding saturated sodium chloride solution to the scale, standing for layering, taking supernatant, filtering with a 0.45 mu m filter membrane, and taking filtrate.
4. Preparation of reference solutions
The medicinal oleum Sesami mainly contains methyl palmitate, methyl stearate, methyl elaidic acid, methyl oleate, methyl linoleate, methyl arachidate, cis-11-eicosenoic acid methyl ester, methyl linolenate, methyl behenate, and methyl lignocerate. Through experimental studies, methyl stearate with stable peak time and moderate peak area was selected as a reference sample provided by Beijing Tanzhong ink quality testing Co., Ltd. (batch No. 0601904 for content measurement).
5. Establishment of detection method
5.1 instruments, reagents and chromatographic conditions
The instrument comprises the following steps: agilent 7890A gas chromatography; agilent GC chromatography workstation.
Reagent: n-heptane was chromatographically pure (Spectrum), water was ultrapure water, and the remaining reagents were analytically pure.
Carrier gas and flow rate: the nitrogen flow rate is to be investigated; sample inlet temperature: 270 ℃; the sample amount is 1 mul; tail blowing: 30 ml/min;
a detector: detector Temperature (TD)280 ℃; a hydrogen Flame Ionization Detector (FID); the hydrogen flow rate was 30ml/min and the air flow rate was 400 ml/min.
5.2 selection of chromatography columns
The influence of capillary chromatographic columns with different polarities on the peak appearance time, the peak area, the peak type, the analysis time and the like of the sesame oil fingerprint spectrum is respectively considered, and the capillary chromatographic columns comprise: firstly, non-polarity: DB-1(30m × 0.25mm × 0.25 μm); low polarity: inter Cap 5(30 m.times.0.25 mm.times.0.25 μm); third, medium polarity: HP-35(30 m.times.0.32 mm.times.0.25 μm); polarity: DB-WAX (30 m.times.0.32 mm. times.0.25 μm); strong polarity: SP-2560(100m multiplied by 0.25mm multiplied by 0.2 μm) shows that the strong polarity chromatographic column SP-2560(100m multiplied by 0.25mm multiplied by 0.2 μm) has better peak output time, peak separation degree and peak type, so the strong polarity chromatographic column SP-2560 is finally determined to be selected.
5.3 selection of the flow Rate of the Carrier gas
The nitrogen flow rates are respectively 0.5, 1.0 and 2.0ml/min, and the influence of the three flow rates on the peak emergence time, the peak area, the peak type, the analysis time and the like of the medicinal sesame oil fingerprint is respectively considered, and the result shows that when the nitrogen flow rate is 1.0ml/min, the peak emergence time and the peak separation degree are also good, the integral analysis time is reasonable within 60min, and therefore the nitrogen flow rate is finally determined to be 1.0 ml/min.
5.4 optimization of temperature Programming
The following temperature programming method is respectively adopted to investigate the fingerprint spectrum of the medicinal sesame oil.
Firstly, the initial temperature is 100 ℃, the temperature is kept for 13min, the temperature is increased to 180 ℃ at the speed of 10 ℃/min, the temperature is kept for 6min, the temperature is increased to 200 ℃ at the speed of 0.5 ℃/min, the temperature is kept for 5min, the temperature is increased to 230 ℃ at the speed of 1 ℃/min, and the temperature is kept for 10.5 min.
② the initial temperature is 60 ℃, the temperature is kept constant for 1min, the temperature is increased to 120 ℃ at 5 ℃/min, the temperature is continuously increased to 200 ℃ at 8 ℃/min, the temperature is further increased to 260 ℃ at 10 ℃/min, and the temperature is kept for 8 min.
③ the initial temperature is 120 ℃, the temperature is kept constant for 1min, the temperature is increased to 170 ℃ at the speed of 6.5 ℃/min, the temperature is increased to 230 ℃ at the speed of 2.75 ℃/min, and the temperature is kept for 12 min.
The result is that the time of the peak appearance and the separation degree of the peak are better when the method is used for programming, and the number of the peaks is more in the analysis time, so the method for finally determining the programming temperature is that the initial temperature is 100 ℃, the temperature is kept for 13min, the temperature is increased to 180 ℃ at 10 ℃/min, the temperature is kept for 6min, the temperature is increased to 200 ℃ at 0.5 ℃/min, the temperature is kept for 5min, the temperature is increased to 230 ℃ at 1 ℃/min, and the temperature is kept for 10.5 min.
5.5 Split ratio selection
Selecting a split flow method for sample injection, setting the split flow ratio as 20:1, 60:1 and 90:1, and respectively inspecting the peak emergence time, the peak area, the peak type, the analysis time and the response value of the medicinal sesame oil fingerprint, wherein the result shows that the peak emergence time, the peak type and the separation degree of the peak are better when the split flow ratio is 60:1, the number of the peaks is more and the response value is proper, so that the split flow ratio is finally determined as 60: 1.
5.6 identification of main chromatographic peaks in the gas chromatography fingerprint of medicinal sesame oil
The main chromatographic peaks in the finished chromatogram can be assigned according to the retention time with the standard: s is methyl stearate, No. 1 is methyl palmitate, No. 2 is methyl palmitate, No. 3 is methyl elaeate, No. 4 is methyl oleate, No. 5 is methyl linoleate, No. 6 is methyl arachinate, No. 7 is methyl cis-11-eicosenoic acid, No. 8 is methyl linolenate, No. 9 is methyl behenate, and No. 10 is methyl lignocerate. Under the fingerprint spectrum measuring condition, the measured fingerprint spectrum of the medicinal sesame oil can reflect the main characteristic components of the medicinal sesame oil.
6. Verification of detection method
6.1 method repeatability test
6 parts of test solution were prepared in parallel according to step 3 from the medicinal sesame oil of lot No. 2-2001018, and the results were shown in tables 1 and 2.
TABLE 1 repeatability test results of gas phase finger print of medicinal sesame oil
(relative retention time of major peaks)
TABLE 2 repeatability test results of gas phase finger print of medicinal sesame oil
(relative peak area of main peak)
The results show that the test method has good repeatability.
6.2 sample stability test
Medicinal sesame oil of batch No. 2-2001018 was prepared in parallel according to step 3, and stability was checked at 0, 3, 6, 9, 12, 24, 36, and 48h for 8 times, and the results are shown in tables 3 and 4.
TABLE 3 stability test results of gas-phase finger-print for medicinal sesame oil
(relative retention time of major peaks)
TABLE 4 stability test results of gas-phase finger-print for medicinal sesame oil
(relative peak area of main peak)
The result shows that the retention time of all the common peaks in the test solution is basically consistent with the peak area of the main peak (accounting for more than 5 percent of the total peak area) (RSD is less than 1 percent), the similarity of the fingerprints obtained by 7 times of sample injection is calculated by using the fingerprint obtained by the 1 st sample injection as the reference and using the traditional Chinese medicine chromatogram fingerprint similarity evaluation system (2012.130723 version, published by the national pharmacopoeia committee), the result similarity accords with the technical requirements of the fingerprints, and the test solution can be stably measured within 48 hours.
The result of the methodology investigation shows that the method for measuring the fingerprint of the medicinal sesame oil has good sample stability and method repeatability, and can accurately measure the fingerprint of the product.
7. Obtaining standard fingerprint spectrum of medicinal sesame oil and determining similar limit
7.120 measurement of batch production finished product and acquisition of standard fingerprint
20 batches of finished products are all produced by Tianjin Da Rentang Jingwanhong pharmaceutical Co Ltd, and the batch numbers are respectively: 2-2001010, 2-2001011, 2-2001012, 2-2001013, 2-2001014, 2-2001015, 2-2001016, 2-2001017, 2-2001018, 2-2001019, 2-2003020, 2-2003021, 2-2003022, 2-2003023, 2-2003024, 2-2003025, 2-2003026, 2-2003027, 2-2003028 and 2-2003029.
Preparing a sample solution according to the step 3, and measuring gas-phase fingerprint spectrum superposition spectrums of 20 batches of finished products according to a method; obtaining standard fingerprints based on 20 batches of finished product fingerprints by using a traditional Chinese medicine chromatogram fingerprint similarity evaluation system; and manually calculating to obtain a standard fingerprint.
7.2 determination of similarity limits of medicinal sesame oils
The similarity of the fingerprints of each batch of finished products is calculated by a traditional Chinese medicine chromatogram fingerprint similarity evaluation system by taking the standard fingerprints of the medicinal sesame oil generated by the similarity calculation software as reference, and the result similarity is more than 0.90 (see table 5). According to the actual production, in order to effectively and comprehensively control the product quality, the similarity between the fingerprint of the specified medicinal sesame oil and the standard fingerprint is calculated by similarity software, and the similarity is more than 0.90.
Table 520 shows the similarity of finger prints of medicinal sesame oil batches
7.3 determination of relative retention time of each characteristic peak and fluctuation range of relative peak area in medicinal sesame oil fingerprint
And (3) importing the obtained detection data of 20 batches of finished product fingerprints into EXCEL, calculating the relative retention time and the relative peak area of each characteristic peak and a reference peak, and obtaining the detection results shown in tables 6 and 7.
Table 620 batch medicinal sesame oil fingerprint relative retention time detection results
Note: s is a reference peak
Table 720 batch medicinal sesame oil fingerprint spectrum relative peak area detection results
Note: s is a reference peak
The average value of the relative retention time and the relative peak area of each characteristic peak in 20 batches of finished fingerprint is respectively used as the relative retention time and the relative peak area value of each characteristic peak of the standard fingerprint, and the fluctuation range of the relative retention time and the relative peak area of each characteristic peak is limited according to the actual production in order to effectively and comprehensively control the product quality, which is shown in tables 8 and 9.
TABLE 8 Standard fingerprint data for medicinal sesame oil
Note: s is a reference peak
TABLE 9 fluctuation range of standard fingerprint relative retention time and relative peak area of medicinal oleum Sesami
Note: s is a reference peak
8. Preliminary investigation of medicinal sesame oil fingerprint stability
The standard fingerprints are used as reference, a traditional Chinese medicine chromatogram fingerprint similarity evaluation system is used for inspecting the fingerprint similarity change conditions of 10 batches of medicinal sesame oil so as to verify the stability, and the results are shown in a table 10.
Table 1010 batches of medicinal sesame oil room temperature sample retention fingerprint spectrum similarity stability investigation results
Test results show that the medicinal sesame oil has little change of fingerprint within 12 months after being kept at room temperature, the similarity is more than 0.99, and the product quality is proved to be stable, and the fingerprint standard can effectively control the quality of finished products.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and should not be taken as limiting the invention, so that any modifications, equivalents, improvements and the like, which are within the spirit and principle of the present invention, should be included in the scope of the present invention.
Claims (7)
1. A fingerprint spectrum detection method of medicinal sesame oil is characterized in that: comprises at least one of methyl palmitate, methyl stearate, methyl elactoate, methyl oleate, methyl linoleate, methyl arachidate, cis-11-eicosenoic acid methyl ester, methyl linolenate, methyl behenate and methyl lignocerate as an effective component, and at least one process of gas chromatography content determination and gas chromatography fingerprint construction is carried out by using the effective component.
2. The method for detecting the fingerprint spectrum of the medicinal sesame oil according to claim 1, which is characterized in that: the gas chromatography conditions were: using a strong polarity capillary chromatography column; carrier gas: nitrogen with flow rate of 0.5-2.0 ml/min; vaporization chamber temperature: 300 ℃ to 330 ℃; the sample amount is 0.1-0.5 mul; tail blowing: 40-60 ml/min; split-flow sampling with split-flow ratio (50-70) 1; a detector: a hydrogen flame ionization detector with the temperature of 250-280 ℃; the hydrogen flow rate is 30-50ml/min, and the air flow rate is 300-500 ml/min; temperature programming: the initial temperature is 90-110 ℃, the temperature is kept constant for 10-15min, the temperature is increased to 180 ℃ at 10 ℃/min, the temperature is kept constant for 5-10min, the temperature is increased to 200 ℃ at 0.5 ℃/min, the temperature is kept constant for 5-10min, the temperature is increased to 230 ℃ at 1 ℃/min, and the temperature is kept constant for 8-12 min.
3. The method for detecting the fingerprint spectrum of the medicinal sesame oil according to claim 1 or 2, which is characterized in that: the gas chromatography conditions were: using a strong polarity capillary chromatography column; carrier gas: nitrogen gas; flow rate: 1 ml/min; a detector: detector Temperature (TD)280 ℃; a hydrogen Flame Ionization Detector (FID); the hydrogen flow rate was 30ml/min and the air flow rate was 400 ml/min. Sample inlet temperature: 320 ℃; the sample amount is 1 mul; tail blowing: 30 ml/min; a hydrogen Flame Ionization Detector (FID); the split ratio is 60: 1; temperature programming: the initial temperature is 100 ℃, the temperature is kept for 13min, the temperature is increased to 180 ℃ at the speed of 10 ℃/min, the temperature is kept for 6min, the temperature is increased to 200 ℃ at the speed of 0.5 ℃/min, the temperature is kept for 5min, the temperature is increased to 230 ℃ at the speed of 1 ℃/min, and the temperature is kept for 10.5 min.
4. The method for detecting the fingerprint spectrum of the medicinal sesame oil according to claim 1, which is characterized in that: the relative retention time of methyl palmitate to methyl stearate is 0.84-0.86, the relative retention time of methyl palmitate to methyl stearate is 0.88-0.91, the relative retention time of methyl elactoate to methyl stearate is 1.03-1.05, the relative retention time of methyl oleate to methyl stearate is 1.05-1.07, the relative retention time of methyl linoleate to methyl stearate is 1.15-1.17, the relative retention time of methyl arachidate to methyl stearate is 1.18-1.20, the relative retention time of methyl cis-11-eicosenoate to methyl stearate is 1.25-1.27, the relative retention time of methyl linolenate to methyl stearate is 1.27-1.29, the relative retention time of methyl behenate to methyl stearate is 1.43-1.45, and the relative retention time of methyl lignocerate to methyl stearate is 1.73-1.75.
5. The method for detecting the fingerprint spectrum of the medicinal sesame oil according to claim 1 or 4, characterized in that: the relative retention time of methyl palmitate to methyl stearate was 0.85, the relative retention time of methyl palmitate to methyl stearate was 0.90, the relative retention time of methyl elactoate to methyl stearate was 1.04, the relative retention time of methyl oleate to methyl stearate was 1.06, the relative retention time of methyl linoleate to methyl stearate was 1.16, the relative retention time of methyl arachidate to methyl stearate was 1.19, the relative retention time of methyl cis-11-eicosanoate to methyl stearate was 1.26, the relative retention time of methyl linolenate to methyl stearate was 1.28, the relative retention time of methyl behenate to methyl stearate was 1.44, and the relative retention time of methyl lignocerate to methyl stearate was 1.74.
6. The method for detecting the fingerprint spectrum of the medicinal sesame oil according to claim 1, which is characterized in that: the relative peak area of methyl palmitate relative to methyl stearate is 1.7-1.8, the relative peak area of methyl palmitate relative to methyl stearate is 0.01-0.03, the relative peak area of methyl elactoate relative to methyl stearate is 0.03-0.06, the relative peak area of methyl oleate relative to methyl stearate is 7.1-7.4, the relative peak area of methyl linoleate relative to methyl stearate is 9.00-9.20, the relative peak area of methyl arachidate relative to methyl stearate is 0.10-0.20, the relative peak area of cis-11-eicosenoic acid methyl ester relative to methyl stearate is 0.02-0.06, the relative peak area of methyl linolenate relative to methyl stearate is 0.04-0.08, the relative peak area of methyl behenate relative to methyl stearate is 0.01-0.05, and the relative peak area of methyl lignocerate relative to methyl stearate is 0.01-0.04.
7. The method for detecting the fingerprint spectrum of the medicinal sesame oil according to claim 1 or 6, which is characterized in that: the relative peak area of methyl palmitate relative to methyl stearate is 1.75, the relative peak area of methyl palmitate relative to methyl stearate is 0.02, the relative peak area of methyl elactoate relative to methyl stearate is 0.05, the relative peak area of methyl oleate relative to methyl stearate is 7.27, the relative peak area of methyl linoleate relative to methyl stearate is 9.07, the relative peak area of methyl arachidate relative to methyl stearate is 0.11, the relative peak area of cis-11-eicosanoenoic acid methyl ester relative to methyl stearate is 0.04, the relative peak area of methyl linolenate relative to methyl stearate is 0.06, the relative peak area of methyl behenate relative to methyl stearate is 0.03, and the relative peak area of methyl lignocerate relative to methyl stearate is 0.02.
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| US20190201471A1 (en) * | 2016-09-09 | 2019-07-04 | Shijiazhuang Yiling Pharmaceutical Co., Ltd. | Usage of semen ziziphi spinosae oil in the treatment of medicinal insomnia |
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