CN113624855B - Method for detecting residual quantity of n-hexane and acetone solvents in crystal lycopene - Google Patents
Method for detecting residual quantity of n-hexane and acetone solvents in crystal lycopene Download PDFInfo
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Abstract
The invention discloses a method for detecting the residual quantity of solvents of n-hexane and acetone in crystal lycopene, which comprises the following steps: s1, crushing crystalline lycopene by using an ultrafine crusher, and uniformly mixing for 5min; s2, taking a uniformly mixed sample of 0.3000+/-0.01 g to 20mL headspace bottle, and adding dichloromethane of chromatographic grade or above for vortex dissolution; s3, adding the solution obtained in the step S2 into N, N-dimethylformamide with chromatographic grade and above, rapidly covering and sealing, heating, performing vortex extraction, standing until layering is complete, and taking the upper layer to be tested; s4, placing the solution obtained in the step S3 into a gas chromatograph headspace sampler, balancing at 80 ℃ for 30min, sucking 1mL of upper gas, and detecting the residual quantity of the n-hexane and acetone solvent by a gas chromatograph-hydrogen ion flame detector.
Description
Technical Field
The invention relates to a method for detecting residual quantity of n-hexane and acetone solvents in crystal lycopene, belonging to the technical field of inspection and detection.
Background
Lycopene (Lycopene) is a natural carotenoid, mainly found in ripe fruits such as tomatoes, watermelons, guava, rosehips, papaya and grapefruits. The molecular structure of the carotenoid is a straight-chain hydrocarbon, is also carotenoid without oxygen elements, is composed of 11 conjugated C=C and two unconjugated C=C, and can efficiently quench singlet oxygen, remove peroxy free radicals, regulate intercellular communication, enhance immunity, regulate cholesterol synthesis and the like. In addition, lycopene can also be used for preventing and treating atherosclerosis, cardiovascular diseases, cancer, etc. Lycopene has been identified as a type a nutrient by the world food and agriculture organization/world health organization (FAO/WHO) and the Joint Expert Committee for Food Additives (JECFA), and has been widely used in the fields of pharmaceutical materials, health products, food additives, cosmetics, and the like. In addition, lycopene has advantages in improving animal health and improving animal product quality.
The crystal lycopene is obtained by crystallization and purification of lycopene oleoresin, the lycopene oleoresin is an oily substance obtained by taking tomatoes and products thereof as raw materials, extracting with organic solvents and removing the organic solvents in the extracting solution, and the lycopene is more than 6-20% by mass, cannot be directly eaten or used for medicines, and can be used in health-care foods, medicines and cosmetics only by purification treatment. Research on the piano and the like shows that the antioxidation effect of the lycopene crystal is superior to that of lycopene oleoresin. The national standard prescribes that the residual quantity of n-hexane and ethyl acetate in lycopene is 50mg/kg, and foreign clients also require that the acetone residual quantity of high-end lycopene is below 200mg/kg, so that the establishment of a solvent residual quantity detection method suitable for n-hexane and acetone in lycopene crystals is significant for the healthy development of the lycopene industry.
At present, the detection method of the solvent residue in the tomato red comprises the following steps: the detection method of the residual amount of normal hexane is water-added wetting detection, the detection method of the residual amount of ethyl acetate is diethyl phthalate extraction detection, the simultaneous detection method of ethyl acetate and ethanol in lycopene oleoresin is dimethyl sulfoxide and water extraction, no report is given on the detection method of the residual amount of acetone in lycopene, and the detection method of the residual amount of normal hexane is not suitable for crystalline lycopene.
The crystal lycopene is a dark red needle crystal, the molecular structure is a linear hydrocarbon, and is also carotenoid without oxygen element, the crystal lycopene is dissolved in chloroform, benzene and grease, and is insoluble in common solvents for detecting solvent residues such as polar solvents DMA, DMF, dimethyl sulfoxide and the like, if the common solvents for detecting solvent residues are used for detecting, the sample is seriously agglomerated at the bottom in the process, the dissolution of n-hexane and acetone solvents is seriously influenced, the residual quantity of n-hexane and acetone in the crystal lycopene can not be accurately detected, the bulk density of the crystal lycopene is smaller according to national standard GB5009.262 detection, and the national standard sampling quantity of 5g occupies more than 10mL in a 20mL headspace bottle and can not be detected.
Therefore, the establishment of a method for reliably and accurately detecting the residual quantity of n-hexane and acetone in the crystal lycopene is a problem to be solved.
Disclosure of Invention
The invention aims to provide a method for detecting the residual quantity of n-hexane and acetone in crystal lycopene, which can reliably and accurately detect the residual quantity of n-hexane and acetone in crystal lycopene only by solving the problem that the residual quantity of n-hexane and acetone in crystal lycopene is difficult to fully extract.
In order to solve the technical problems, the invention adopts the following technical scheme:
a method for detecting the residual quantity of n-hexane and acetone solvents in crystal lycopene comprises the following steps:
s1, crushing crystalline lycopene by using an ultrafine crusher, and uniformly mixing for 5min;
s2, taking a uniformly mixed sample of 0.3000+/-0.01 g to 20mL headspace bottle, and adding dichloromethane of chromatographic grade or above for vortex dissolution;
s3, adding the solution obtained in the step S2 into N, N-dimethylformamide with chromatographic grade and above, rapidly covering and sealing, heating, performing vortex extraction, standing until layering is complete, and taking the upper layer to be measured;
s4, placing the solution obtained in the step S3 into a gas chromatograph headspace sampler, balancing at 80 ℃ for 30min, sucking 1mL of upper gas, and detecting the residual quantity of the n-hexane and acetone solvent by a gas chromatograph-hydrogen ion flame detector.
The technical scheme of the invention is further improved as follows: in the step S1, the crushing end point is that the passing rate of a 100-mesh sieve reaches more than 95 percent.
The technical scheme of the invention is further improved as follows: the addition amount of the methylene dichloride in the step S2 is 0.2-1 mL.
The technical scheme of the invention is further improved as follows: the addition amount of N, N-dimethylformamide in the step S3 is 5-5.8 mL.
The technical scheme of the invention is further improved as follows: and the heating temperature in the step S3 is 50-60 ℃, the heating time is 10min, and the vortex extraction is carried out for 3-5 min.
The technical scheme of the invention is further improved as follows: and in the step S3, the standing temperature is 20-25 ℃, and the standing time is 10-20 min.
The technical scheme of the invention is further improved as follows: the gas chromatography condition in the step S4 is a chromatographic column polyethylene glycol nitrobenzene modified capillary column, the column length is 60m, the column inner diameter is 0.25mm, the film thickness is 0.25 mu m, the carrier gas is nitrogen, the flow rate is 3.0mL/min, the sample inlet temperature is 220 ℃, the column temperature is programmed temperature, the detector temperature is 235 ℃, and the split ratio is 25:1.
The technical scheme of the invention is further improved as follows: the temperature programming condition is that the initial temperature is 60 ℃, the temperature is kept for 5min, the temperature is increased to 85 ℃ at 3.5 ℃/min, and then the temperature is increased to 220 ℃ at 20 ℃/min, and the temperature is kept for 1min.
The technical scheme of the invention is further improved as follows: the quantitative mode is an external standard curve method, 5-5.8 mL of N, N-dimethylformamide is taken as a matrix, and n-hexane and acetone standard substances are respectively added to prepare a series of standard solutions of 0, 2, 5, 10, 20 and 50 mg/L.
By adopting the technical scheme, the invention has the following technical progress:
the invention can accurately detect the residual quantity of normal hexane and acetone in the crystal lycopene; the method is simple to operate, accurate and reliable in result and good in reproducibility; technical assurance is provided for producing and selling the crystal lycopene with controlled residual amount of n-hexane and acetone solvent and the crystal lycopene used by customers, and technical support is provided for subsequent research of acetone production mechanism.
Detailed Description
The invention is further illustrated by the following examples:
a method for detecting the residual quantity of n-hexane and acetone solvents in crystal lycopene comprises the following steps:
s1, crushing the crystal lycopene by using an ultrafine crusher until the passing rate of a 100-mesh sieve reaches more than 95%, and uniformly mixing for 5min;
s2, taking a uniformly mixed sample of 0.3000+/-0.01 g to 20mL of headspace bottle, and adding 0.2-1 mL of dichloromethane with chromatographic grade and above for vortex dissolution;
s3, adding 5-5.8 mL of N, N-dimethylformamide with chromatographic grade and above grade into the solution obtained in the step S2, rapidly capping and sealing, heating to 50-60 ℃ for 10min, performing vortex extraction for 3-5 min, standing at 20-25 ℃ for 10-20 min until layering is complete, and taking the upper layer to be detected;
s4, placing the solution obtained in the step S3 into a gas chromatograph headspace sampler, balancing at 80 ℃ for 30min, sucking 1mL of upper gas, and detecting the residual quantity of the n-hexane and acetone solvent by a gas chromatograph-hydrogen ion flame detector.
The gas chromatography condition is chromatographic column polyethylene glycol nitrobenzene modified capillary column, the column length is 60m, the column inner diameter is 0.25mm, the film thickness is 0.25 μm, the carrier gas is nitrogen, the flow is 3.0mL/min, the sample inlet temperature is 220 ℃, the column temperature is programmed temperature, the detector temperature is 235 ℃, and the split ratio is 25:1. The temperature programming condition is that the initial temperature is 60 ℃, the temperature is kept for 5min, the temperature is increased to 85 ℃ at 3.5 ℃/min, and then the temperature is increased to 220 ℃ at 20 ℃/min, and the temperature is kept for 1min.
The quantitative mode is an external standard curve method, 5-5.8 mL of N, N-dimethylformamide solvent is taken as a matrix, and n-hexane and acetone standard substances are respectively added to prepare a series of standard solutions of 0, 2, 5, 10, 20 and 50 mg/L.
Example 1
Pulverizing crystal lycopene with superfine pulverizer until the passing rate of 100 mesh sieve reaches above 95%, and mixing for 5min; taking a uniformly mixed sample, adding 0.3000+/-0.01 g to 20mL of dichloromethane with a chromatographic grade of 0.5mL and above into a headspace bottle, and vortex dissolving; adding 5.5mL of chromatographic grade and above grade N, N-Dimethylformamide (DMF), rapidly covering and sealing, heating at 55deg.C for 10min, extracting by vortex for 4min, standing at 22deg.C for 10min, layering completely, and collecting the upper layer to be detected; putting the lycopene into a gas chromatograph headspace sampler, balancing at 80 ℃ for 30min, sucking 1mL of upper gas, detecting the content of n-hexane and acetone in the crystal lycopene by a gas chromatograph-hydrogen ion flame detector, and detecting samples 1, 2 and 3, wherein the detection results are shown in table 1; the gas chromatography condition is that a chromatographic column polyethylene glycol nitrobenzene modified capillary column has a column length of 60m, a column inner diameter of 0.25mm, a film thickness of 0.25 mu m, carrier gas is nitrogen, the flow rate of the carrier gas is 3.0mL/min, the temperature of a sample inlet is 220 ℃, the temperature of the column is programmed, the temperature of a detector is 235 ℃, and the split ratio is 25:1; the temperature programming condition is that the temperature is initially 60 ℃, the temperature is kept for 3min, the temperature is increased to 85 ℃ at 3.5 ℃/min, and the temperature is increased to 220 ℃ at 20 ℃/min, and the temperature is kept for 1min.
Table 1 example 1 test results table
Example 2
Pulverizing crystal lycopene with superfine pulverizer until the passing rate of 100 mesh sieve reaches above 95%, and mixing for 5min; taking a uniformly mixed sample, adding 0.3000+/-0.01 g to 20mL of dichloromethane with a chromatographic grade of 0.6mL and above into a headspace bottle, and vortex dissolving; adding 5.4mL of chromatographic grade and above grade N, N-Dimethylformamide (DMF), rapidly capping and sealing, heating at 53 ℃ for 10min, performing vortex 5min extraction, standing at 25 ℃ for 15min, layering completely, and taking the upper layer to be detected; putting the lycopene into a gas chromatograph headspace sampler, balancing at 80 ℃ for 30min, sucking 1mL of upper gas, detecting the content of n-hexane and acetone in the crystal lycopene by a gas chromatograph-hydrogen ion flame detector, and detecting samples 1, 2 and 3, wherein the detection results are shown in table 2; the gas chromatography condition is that a chromatographic column polyethylene glycol nitrobenzene modified capillary column has a column length of 60m, a column inner diameter of 0.25mm, a film thickness of 0.25 mu m, carrier gas is nitrogen, the flow rate of the carrier gas is 3.0mL/min, the temperature of a sample inlet is 220 ℃, the temperature of the column is programmed, the temperature of a detector is 235 ℃, and the split ratio is 25:1; the temperature programming condition is that the temperature is initially 60 ℃, the temperature is kept for 3min, the temperature is increased to 85 ℃ at 3.5 ℃/min, and the temperature is increased to 220 ℃ at 20 ℃/min, and the temperature is kept for 1min.
Table 2 example 2 test results table
Example 3
Pulverizing crystal lycopene with superfine pulverizer until the passing rate of 100 mesh sieve reaches above 95%, and mixing for 5min; taking a uniformly mixed sample, adding 0.3000+/-0.01 g to 20mL of dichloromethane with a chromatographic grade of 0.4mL and above into a headspace bottle, and carrying out vortex dissolution; adding 5.6mL of chromatographic grade and above grade N, N-Dimethylformamide (DMF), rapidly capping and sealing, heating at 60deg.C for 10min, extracting by vortex for 4min, standing at 20deg.C for 20min, layering completely, and collecting upper layer to be detected; putting the lycopene into a gas chromatograph headspace sampler, balancing at 80 ℃ for 30min, sucking 1mL of upper gas, detecting the content of n-hexane and acetone in the crystal lycopene by a gas chromatograph-hydrogen ion flame detector, and detecting samples 1, 2 and 3, wherein the detection results are shown in table 3; the gas chromatography condition is that a chromatographic column polyethylene glycol nitrobenzene modified capillary column has a column length of 60m, a column inner diameter of 0.25mm, a film thickness of 0.25 mu m, carrier gas is nitrogen, the flow rate of the carrier gas is 3.0mL/min, the temperature of a sample inlet is 220 ℃, the temperature of the column is programmed, the temperature of a detector is 235 ℃, and the split ratio is 25:1; the temperature programming condition is that the temperature is initially 60 ℃, the temperature is kept for 3min, the temperature is increased to 85 ℃ at 3.5 ℃/min, and the temperature is increased to 220 ℃ at 20 ℃/min, and the temperature is kept for 1min.
Table 3 example 3 test results table
Example 4
Pulverizing crystal lycopene with superfine pulverizer until the passing rate of 100 mesh sieve reaches above 95%, and mixing for 5min; taking a uniformly mixed sample, adding 0.3000+/-0.01 g to 20mL of dichloromethane with a chromatographic grade of 1.0mL and above into a headspace bottle, and vortex dissolving; adding 5.0mL of chromatographic grade and above grade N, N-Dimethylformamide (DMF), rapidly covering and sealing, heating at 57 ℃ for 10min, performing vortex for 3min for extraction, standing at 23 ℃ for 17min, layering completely, and taking the upper layer to be detected; putting the lycopene into a gas chromatograph headspace sampler, balancing at 80 ℃ for 30min, sucking 1mL of upper gas, detecting the content of n-hexane and acetone in the crystal lycopene by a gas chromatograph-hydrogen ion flame detector, and detecting samples 1, 2 and 3, wherein the detection results are shown in Table 4; the gas chromatography condition is that a chromatographic column polyethylene glycol nitrobenzene modified capillary column has a column length of 60m, a column inner diameter of 0.25mm, a film thickness of 0.25 mu m, carrier gas is nitrogen, the flow rate of the carrier gas is 3.0mL/min, the temperature of a sample inlet is 220 ℃, the temperature of the column is programmed, the temperature of a detector is 235 ℃, and the split ratio is 25:1; the temperature programming condition is that the temperature is initially 60 ℃, the temperature is kept for 3min, the temperature is increased to 85 ℃ at 3.5 ℃/min, and the temperature is increased to 220 ℃ at 20 ℃/min, and the temperature is kept for 1min.
Table 4 example 4 test results table
Example 5
Pulverizing crystal lycopene with superfine pulverizer until the passing rate of 100 mesh sieve reaches above 95%, and mixing for 5min; taking a uniformly mixed sample, adding 0.3000+/-0.01 g to 20mL of dichloromethane with a chromatographic grade of 0.2mL and above into a headspace bottle, and vortex dissolving; adding 5.8mL of chromatographic grade and above grade N, N-Dimethylformamide (DMF), rapidly capping and sealing, heating at 50deg.C for 10min, extracting by vortex for 5min, standing at 24deg.C for 13min, layering completely, and collecting the upper layer to be detected; putting the lycopene into a gas chromatograph headspace sampler, balancing at 80 ℃ for 30min, sucking 1mL of upper gas, detecting the content of n-hexane and acetone in the crystal lycopene by a gas chromatograph-hydrogen ion flame detector, and detecting samples 1, 2 and 3, wherein the detection results are shown in Table 5; the gas chromatography condition is that a chromatographic column polyethylene glycol nitrobenzene modified capillary column has a column length of 60m, a column inner diameter of 0.25mm, a film thickness of 0.25 mu m, carrier gas is nitrogen, the flow rate of the carrier gas is 3.0mL/min, the temperature of a sample inlet is 220 ℃, the temperature of the column is programmed, the temperature of a detector is 235 ℃, and the split ratio is 25:1; the temperature programming condition is that the temperature is initially 60 ℃, the temperature is kept for 3min, the temperature is increased to 85 ℃ at 3.5 ℃/min, and the temperature is increased to 220 ℃ at 20 ℃/min, and the temperature is kept for 1min.
Table 5 example 5 test results table
To sum up: in the parallel experiments of the embodiment of the invention on 3 samples, the content of n-hexane and acetone measured by 5 parallel experiments of each sample are similar, and the difference is small, so that the invention can accurately detect the residual quantity of n-hexane and acetone in crystal lycopene, and has accurate and reliable result and good reproducibility.
Comparative example 1 vortex dissolution without addition of dichloromethane
Pulverizing crystal lycopene with superfine pulverizer until the passing rate of 100 mesh sieve reaches above 95%, and mixing for 5min; taking a uniformly mixed sample of 0.3000+/-0.01 g to 20mL of headspace bottle, directly adding 6mL of DMF, and rapidly capping and sealing, and otherwise carrying out the same process as in example 1. The test results are shown in Table 6.
Table 6 comparative example 1 test results table
Comparative example 2 dissolution with a larger amount of dichloromethane without DMF
Pulverizing crystal lycopene with superfine pulverizer until the passing rate of 100 mesh sieve reaches above 95%, and mixing for 5min; taking a uniformly mixed sample of 0.3000+/-0.01 g to 20mL of headspace bottle, adding 6mL of dichloromethane, rapidly capping and sealing, and otherwise carrying out the same process as in example 1. The test results are shown in Table 7.
Table 7 comparative example 2 test results table
Comparative example 3 dissolution with DMA alone
Pulverizing crystal lycopene with superfine pulverizer until the passing rate of 100 mesh sieve reaches above 95%, and mixing for 5min; taking 0.3000+/-0.01 g to 20mL of uniformly mixed sample, adding 6mL of DMA into a headspace bottle, and rapidly capping and sealing, wherein the other steps are the same as in example 1. The test results are shown in Table 8.
Table 8 comparative example 3 test results table
Comparative example 4
Pulverizing crystal lycopene with pulverizer until 80 mesh sieve passing rate reaches above 95%, and mixing for 5min; other steps are as in example 1. The test results are shown in Table 9.
Table 9 comparative example 4 test results table
From the analysis of the results in tables 6 to 9, it can be seen that: the lower content of the n-hexane and the acetone detected in the comparative examples 1 and 3 indicates that the n-hexane and the acetone are not completely dissolved out, and the detection result is inaccurate; comparative examples 2 and 4 detected a large difference in the results of 5 parallel experiments for each sample, indicating that the detection results were inaccurate.
Claims (4)
1. A method for detecting the residual quantity of n-hexane and acetone solvents in crystal lycopene is characterized by comprising the following steps of: the method comprises the following steps:
s1, crushing crystalline lycopene by using an ultrafine crusher, and uniformly mixing for 5min;
s2, taking a uniformly mixed sample of 0.3000+/-0.01 g to 20mL headspace bottle, and adding dichloromethane of chromatographic grade or above for vortex dissolution;
s3, adding the solution obtained in the step S2 into N, N-dimethylformamide with chromatographic grade and above, rapidly covering and sealing, heating, performing vortex extraction, standing until layering is complete, and taking the upper layer to be tested;
s4, placing the solution obtained in the step S3 into a gas chromatograph headspace sampler, balancing at 80 ℃ for 30min, sucking 1mL of upper gas, and detecting the residual quantity of the n-hexane and acetone solvent by a gas chromatograph-hydrogen ion flame detector;
in the step S1, the crushing end point is that the passing rate of a 100-mesh sieve reaches more than 95 percent;
the addition amount of dichloromethane in the step S2 is 0.2-1 mL;
the addition amount of N, N-dimethylformamide in the step S3 is 5-5.8 mL;
the gas chromatography condition in the step S4 is a chromatographic column polyethylene glycol nitrobenzene modified capillary column, the column length is 60m, the column inner diameter is 0.25mm, the film thickness is 0.25 mu m, the carrier gas is nitrogen, the flow rate is 3.0mL/min, the sample inlet temperature is 220 ℃, the column temperature is programmed temperature, the detector temperature is 235 ℃, and the split ratio is 25:1;
the temperature programming condition is that the initial temperature is 60 ℃, the temperature is kept for 5min, the temperature is increased to 85 ℃ at 3.5 ℃/min, and then the temperature is increased to 220 ℃ at 20 ℃/min, and the temperature is kept for 1min.
2. A method for detecting residual solvent content of n-hexane and acetone in crystal lycopene according to claim 1, wherein the method comprises the following steps: and the heating temperature in the step S3 is 50-60 ℃, the heating time is 10min, and the vortex extraction is carried out for 3-5 min.
3. A method for detecting residual solvent content of n-hexane and acetone in crystal lycopene according to claim 1, wherein the method comprises the following steps: and in the step S3, the standing temperature is 20-25 ℃, and the standing time is 10-20 min.
4. A method for detecting residual solvent content of n-hexane and acetone in crystal lycopene according to claim 1, wherein the method comprises the following steps: the quantitative mode is an external standard curve method, 5-5.8 mL of N, N-dimethylformamide is taken as a matrix, and n-hexane and acetone standard substances are respectively added to prepare a series of standard solutions of 0, 2, 5, 10, 20 and 50 mg/L.
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| US5965183A (en) * | 1994-10-31 | 1999-10-12 | Hartal; Dov | Stable lycopene concentrates and process for their preparation |
| US8449911B2 (en) * | 2003-03-12 | 2013-05-28 | Takeda Pharmaceutical Company Limited | Drug composition having active ingredient adhered at high concentration to spherical core |
| CN1326836C (en) * | 2006-02-23 | 2007-07-18 | 上海交通大学 | Lycopene purification preparation method |
| AU2013200516B2 (en) * | 2006-07-12 | 2015-09-03 | University Of Tennessee Research Foundation | Substituted Acylanilides and Methods of Use Thereof |
| EP2103309A3 (en) * | 2008-03-19 | 2012-09-12 | SCHWEIGERT, Florian | Method for extracting and proving soluble fat materials from biological materials |
| CN102267881B (en) * | 2010-06-02 | 2013-07-24 | 绍兴文理学院 | Lycopene intermediate and preparation method thereof |
| WO2013002398A1 (en) * | 2011-06-30 | 2013-01-03 | 株式会社カネカ | Method for producing carotenoid composition |
| WO2013041935A1 (en) * | 2011-09-19 | 2013-03-28 | Omniactive Health Technologies Limited | An efficient process for the preparation of lycopene containing oleoresin and lycopene crystals for human consumption |
| CN106198819B (en) * | 2016-08-30 | 2018-08-21 | 南京正大天晴制药有限公司 | The method of residual solvent in Headspace Gas Chromatography Xi Gelieting bulk pharmaceutical chemicals |
| CN107361259B (en) * | 2017-07-17 | 2020-11-17 | 北京市农林科学院 | A method for preparing tomato juice rich in pectin oligosaccharide and lycopene with high bioavailability |
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