CN110333213A - The detection method of benzoate and sorbate in a kind of food - Google Patents
The detection method of benzoate and sorbate in a kind of food Download PDFInfo
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- CN110333213A CN110333213A CN201810960816.7A CN201810960816A CN110333213A CN 110333213 A CN110333213 A CN 110333213A CN 201810960816 A CN201810960816 A CN 201810960816A CN 110333213 A CN110333213 A CN 110333213A
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- benzoate
- sorbate
- detection method
- organic solvent
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- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 238000001514 detection method Methods 0.000 title claims abstract description 35
- WSWCOQWTEOXDQX-MQQKCMAXSA-M (E,E)-sorbate Chemical compound C\C=C\C=C\C([O-])=O WSWCOQWTEOXDQX-MQQKCMAXSA-M 0.000 title claims abstract description 32
- 229940075554 sorbate Drugs 0.000 title claims abstract description 32
- 235000013305 food Nutrition 0.000 title claims abstract description 28
- 239000003960 organic solvent Substances 0.000 claims abstract description 19
- 239000007788 liquid Substances 0.000 claims abstract description 18
- 238000013517 stratification Methods 0.000 claims abstract description 13
- 238000001069 Raman spectroscopy Methods 0.000 claims abstract description 12
- 150000007524 organic acids Chemical class 0.000 claims abstract description 10
- 150000003839 salts Chemical class 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical group O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000007787 solid Substances 0.000 claims abstract description 7
- 239000012530 fluid Substances 0.000 claims abstract description 6
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 21
- 239000000243 solution Substances 0.000 claims description 16
- 235000010199 sorbic acid Nutrition 0.000 claims description 14
- BEFDCLMNVWHSGT-UHFFFAOYSA-N ethenylcyclopentane Chemical compound C=CC1CCCC1 BEFDCLMNVWHSGT-UHFFFAOYSA-N 0.000 claims description 13
- 239000004334 sorbic acid Substances 0.000 claims description 13
- 229940075582 sorbic acid Drugs 0.000 claims description 13
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 7
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 6
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 6
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 6
- 238000004416 surface enhanced Raman spectroscopy Methods 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 4
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 4
- 239000003208 petroleum Substances 0.000 claims description 4
- 239000000284 extract Substances 0.000 claims description 3
- -1 halide salt Chemical class 0.000 claims description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 2
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 2
- 229910019142 PO4 Inorganic materials 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 claims description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 2
- 239000010452 phosphate Substances 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims description 2
- 238000004445 quantitative analysis Methods 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims 2
- 230000016615 flocculation Effects 0.000 claims 1
- 238000005189 flocculation Methods 0.000 claims 1
- 238000001228 spectrum Methods 0.000 claims 1
- 239000012153 distilled water Substances 0.000 abstract 1
- 239000005711 Benzoic acid Substances 0.000 description 10
- 235000010233 benzoic acid Nutrition 0.000 description 10
- 238000000605 extraction Methods 0.000 description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 230000010355 oscillation Effects 0.000 description 9
- 239000006228 supernatant Substances 0.000 description 7
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 5
- 235000013361 beverage Nutrition 0.000 description 5
- 235000013399 edible fruits Nutrition 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 239000001103 potassium chloride Substances 0.000 description 4
- 235000011164 potassium chloride Nutrition 0.000 description 4
- 239000003755 preservative agent Substances 0.000 description 4
- 230000002335 preservative effect Effects 0.000 description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 239000000796 flavoring agent Substances 0.000 description 3
- 235000019634 flavors Nutrition 0.000 description 3
- 210000002216 heart Anatomy 0.000 description 3
- 235000015094 jam Nutrition 0.000 description 3
- 235000013622 meat product Nutrition 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 description 3
- 239000004299 sodium benzoate Substances 0.000 description 3
- 235000010234 sodium benzoate Nutrition 0.000 description 3
- 235000013555 soy sauce Nutrition 0.000 description 3
- 235000005979 Citrus limon Nutrition 0.000 description 2
- 244000131522 Citrus pyriformis Species 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- QIAFMBKCNZACKA-UHFFFAOYSA-N N-benzoylglycine Chemical compound OC(=O)CNC(=O)C1=CC=CC=C1 QIAFMBKCNZACKA-UHFFFAOYSA-N 0.000 description 2
- 238000001237 Raman spectrum Methods 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 235000011389 fruit/vegetable juice Nutrition 0.000 description 2
- 235000015110 jellies Nutrition 0.000 description 2
- 239000008274 jelly Substances 0.000 description 2
- 230000003907 kidney function Effects 0.000 description 2
- 210000004185 liver Anatomy 0.000 description 2
- 235000011475 lollipops Nutrition 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000020477 pH reduction Effects 0.000 description 2
- 235000015277 pork Nutrition 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000001988 toxicity Effects 0.000 description 2
- 231100000419 toxicity Toxicity 0.000 description 2
- 238000002137 ultrasound extraction Methods 0.000 description 2
- 235000021419 vinegar Nutrition 0.000 description 2
- 239000000052 vinegar Substances 0.000 description 2
- FTLYMKDSHNWQKD-UHFFFAOYSA-N (2,4,5-trichlorophenyl)boronic acid Chemical compound OB(O)C1=CC(Cl)=C(Cl)C=C1Cl FTLYMKDSHNWQKD-UHFFFAOYSA-N 0.000 description 1
- 208000010444 Acidosis Diseases 0.000 description 1
- 240000007154 Coffea arabica Species 0.000 description 1
- 206010010904 Convulsion Diseases 0.000 description 1
- 235000009917 Crataegus X brevipes Nutrition 0.000 description 1
- 235000013204 Crataegus X haemacarpa Nutrition 0.000 description 1
- 235000009685 Crataegus X maligna Nutrition 0.000 description 1
- 235000009444 Crataegus X rubrocarnea Nutrition 0.000 description 1
- 235000009486 Crataegus bullatus Nutrition 0.000 description 1
- 235000017181 Crataegus chrysocarpa Nutrition 0.000 description 1
- 235000009682 Crataegus limnophila Nutrition 0.000 description 1
- 235000004423 Crataegus monogyna Nutrition 0.000 description 1
- 240000000171 Crataegus monogyna Species 0.000 description 1
- 235000002313 Crataegus paludosa Nutrition 0.000 description 1
- 235000009840 Crataegus x incaedua Nutrition 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 206010020751 Hypersensitivity Diseases 0.000 description 1
- 206010027417 Metabolic acidosis Diseases 0.000 description 1
- 241000220324 Pyrus Species 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 244000269722 Thea sinensis Species 0.000 description 1
- 208000024780 Urticaria Diseases 0.000 description 1
- 208000026935 allergic disease Diseases 0.000 description 1
- 230000007815 allergy Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 208000006673 asthma Diseases 0.000 description 1
- 235000013527 bean curd Nutrition 0.000 description 1
- WXBLLCUINBKULX-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1.OC(=O)C1=CC=CC=C1 WXBLLCUINBKULX-UHFFFAOYSA-N 0.000 description 1
- 229960004365 benzoic acid Drugs 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000036772 blood pressure Effects 0.000 description 1
- 235000008429 bread Nutrition 0.000 description 1
- 235000014171 carbonated beverage Nutrition 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 235000016213 coffee Nutrition 0.000 description 1
- 235000013353 coffee beverage Nutrition 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000036461 convulsion Effects 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- 235000013365 dairy product Nutrition 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000012259 ether extract Substances 0.000 description 1
- XYIBRDXRRQCHLP-UHFFFAOYSA-N ethyl acetoacetate Chemical compound CCOC(=O)CC(C)=O XYIBRDXRRQCHLP-UHFFFAOYSA-N 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 235000021022 fresh fruits Nutrition 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 230000004217 heart function Effects 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 231100000567 intoxicating Toxicity 0.000 description 1
- 230000002673 intoxicating effect Effects 0.000 description 1
- 238000000622 liquid--liquid extraction Methods 0.000 description 1
- 230000003908 liver function Effects 0.000 description 1
- 235000013372 meat Nutrition 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 230000032696 parturition Effects 0.000 description 1
- 235000021017 pears Nutrition 0.000 description 1
- RGSFGYAAUTVSQA-UHFFFAOYSA-N pentamethylene Natural products C1CCCC1 RGSFGYAAUTVSQA-UHFFFAOYSA-N 0.000 description 1
- 125000004817 pentamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 description 1
- 235000021110 pickles Nutrition 0.000 description 1
- 235000021568 protein beverage Nutrition 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 229940085605 saccharin sodium Drugs 0.000 description 1
- 235000015067 sauces Nutrition 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 150000003398 sorbic acids Chemical class 0.000 description 1
- 235000013616 tea Nutrition 0.000 description 1
- YNJBWRMUSHSURL-UHFFFAOYSA-N trichloroacetic acid Chemical compound OC(=O)C(Cl)(Cl)Cl YNJBWRMUSHSURL-UHFFFAOYSA-N 0.000 description 1
- 210000002700 urine Anatomy 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
- G01N21/658—Raman scattering enhancement Raman, e.g. surface plasmons
Landscapes
- Health & Medical Sciences (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention discloses the detection methods of benzoate and sorbate in a kind of food, include the following steps: 1) to weigh appropriate amount of sample, appropriate organic solvent is added to extract, wherein, the mass volume ratio range of solid sample and organic solvent is 1:1~1:10g/mL, and the mass volume ratio range of fluid sample and organic solvent is 1:0.5~1:10g/mL；It is added organic acid in organic solvent in advance, the volume ratio range of organic solvent and organic acid is 10:1~1000:1；It is transferred in separatory funnel after extracting solution is centrifuged, appropriate secondary distilled water is added, vibrated, stratification, lower layer's solution is spare as prepare liquid；2) it takes appropriate prepare liquid in Raman sample bottle, appropriate metal-sol is added and mixes, add suitable inorganic salts flocculant and mix, be then placed on Raman spectrometer detection interior and detected.
Description
Technical field
The present invention relates to the detection methods of benzoate and sorbate in a kind of food.
Background technique
Benzoic acid (Benzoic acid) and sorbic acid (Sorbic acid) are that the currently most used food in China is organic
Preservative is widely used in varieties of food items.Benzoic acid can generate hippuric acid in conjunction with the intracorporal amion acetic acid of people and with urine
It excretes.Such as Excess free enthalpy benzoic acid and benzoate, it will influence effect of the liver enzyme to fatty acid, secondly benzoate
In excessive sodium human blood-pressure, heart, renal function can also be had an impact.Especially weak to heart, Liver and kidney function crowd and
Speech, benzoic acid and ingesting for benzoate are unsuitable.In addition it is sick that metabolic acidosis, convulsions and asthma etc. be there is also
Disease.Benzoic acid and sodium benzoate because have superposition intoxicating phenomenon report, it is disputable in use, though still for various countries allow using,
But application range is more and more narrow.Just limitation uses in the imported food of Japan, or even part is forbidden to use, and Japan has stopped giving birth to
It produces.But it is cheap because being worth, it is still used as main preservative in China.Sorbic acid has lower toxicity, is state so far
The generally acknowledged best preservative in border, has become the mainstream preservative of western developed country.But in fact, now it has been reported that
Many cases (nettle rash and false allergy) illustrate in human body to harm brought by excessive sorbic acid.
According to China GB 2760-2014 " national food safety standard food additives use standard " regulation, jam, vinegar,
The sorbic acids such as soy sauce, Pickle, bean curd dried product, bread, cake and its sylvite maximum usage amount are 1000ppm, beverage class,
Sorbic acid and its sylvite maximum usage amount are 500ppm, cold cuts in flavor ice lolly, surface treated fresh fruit, preserved fruit fruit jelly etc.
Sorbic acid and its sylvite maximum usage amount are 75ppm in product, shortening aquatic products (can directly eat).Flavor ice lolly, jam,
Vinegar, soy sauce, sauce and jam product, semi-solid composite flavor, juice (slurry) class beverage, protein beverage, tea, coffee, plant
Benzoic acid and sodium benzoate maximum usage amount is 1000ppm, benzoic acid and sodium benzoate most ambassador in preserved fruit fruit jelly in (class) beverage etc.
Dosage is 500ppm, and benzoic acid maximum usage amount in soda, specific use beverage is 200ppm.
Domestic detection sorbic acid and benzoic acid are mainly according to GB/T5009.29-2003 " sorbic acid, benzene first in food at present
Acid measurement ", GB/T 21703-2010 " measurement of benzoic acid and sorbic acid in national food safety standard cream and dairy products ",
GB/T 23495-2009 " the measurement high performance liquid chromatography of benzoic acid, sorbic acid and saccharin sodium in food " and SB/T 10389-
2004 " measurements of sorbic acid in meat and meat products ", cardinal principle is that solid is extracted with water, and petroleum ether extracts after hydrochloric acid acidification
It takes；Fluid sample first removes ethyl alcohol and carbon dioxide, and pH value is adjusted to neutrality, removes removing protein；Sorbic acid in meat products is then used
After extraction with aqueous solution, crosses neutral alumina and live to clean.The sample gas-chromatography or liquid chromatographic detection handled well.This is needed
Large-scale instrument and the professional for being familiar with and operating large-scale instrument, and the time is long.
Summary of the invention
The object of the present invention is to provide benzoate and mountains in a kind of food that simple and efficient to handle, achievable scene uses
The detection method of pears hydrochlorate.
Technical scheme is as follows:
The detection method of benzoate and sorbate, includes the following steps: in a kind of food
1) appropriate amount of sample is weighed, appropriate organic solvent is added and extracts, wherein the quality volume of solid sample and organic solvent
It is 1:1~1:10g/mL than range, the mass volume ratio range of fluid sample and organic solvent is 1:0.5~1:10g/mL；Have
It is added organic acid in solvent in advance, the volume ratio range of organic solvent and organic acid is 10:1~1000:1；By extracting solution from
It is transferred in separatory funnel after the heart, appropriate aqueous solution is added, vibrated, stratification, lower layer's solution is spare as prepare liquid；
2) it takes appropriate prepare liquid in Raman sample bottle, appropriate metal-sol is added and mixes, adds suitable inorganic salts
Flocculant mixes, and is then placed on Raman spectrometer detection interior and is detected.
Preferably, in step 1), the organic solvent is petroleum ether, n-hexane, hexamethylene, heptane, methylene chloride, second
Acetoacetic ester or its mixed liquor.
Preferably, organic acid acidification is added in the organic solvent.
Preferably, the organic acid is acetic acid, concentration 0.1%-10%.
Preferably, the aqueous solution is preferably secondary water.
Preferably, the secondary water is alkalinity, pH value 8-13.
Preferably, organic phase extracted is transferred in another separatory funnel in step 1), and appropriate aqueous solution is added, and is shaken
It swings, stratification, lower layer's solution is spare as prepare liquid.
Preferably, the metal-sol is nanogold or nano silver.
Preferably, the inorganic salts flocculant be sulfate, nitrate, carbonate, silicate, acetate, phosphate or
Halide salt.The prepare liquid, metal-sol, inorganic salts flocculant additional amount be the 10 μ L:10 μ L~500 of μ L~200 μ of volume ratio
The L:10 μ μ of L~500 L.
Preferably, step 1) or 2) before, further include standard curve preparation step, the benzene first of mark-on various concentration in food
The feature peak intensity that spiked levels and scanning obtain is drawn standard curve by hydrochlorate and sorbate；Benzoate surface enhanced
The characteristic peak of Raman spectrum is 839cm-1, 1001cm-1, 1023cm-1Or 1597cm-1, sorbate Surface enhanced Raman spectroscopy
Characteristic peak be 1154cm-1, 1377cm-1Or 1642cm-1。
Preferably, detection method of the invention further includes step 3), by the testing result of step 2) and draws standard curve
Comparison, obtains benzoate and sorbate quantitative analysis results in food.
The present invention is acidified organic solvent using organic acid, can dissolve each other with organic solvent, does not need in addition to add acid.Using
The organic solvents such as the petroleum ether of hypotoxicity injure experimenter small.It is applied widely, it is easy to operate quick, within 10min just
Detection while can completing to detect, and can realize sorbate and benzoate is not necessarily to professional, and fluid sample is without pre-
First remove removing carbon dioxide, ethyl alcohol.
The present invention extracts and detection method institute for the Raman detection method of benzoate and sorbate in existing food
Existing deficiency, using Surface enhanced Raman spectroscopy and liquid-liquid extraction, have step is simple, analysis time is short, reagent toxicity is small,
Selectivity is good, do not need professional person, need large-scale instrument, can be achieved the various food in scene, including meat products, various salts down
In product and fluid sample the advantages that the quick and precisely detection of benzoate and sorbate.
Detailed description of the invention
Present invention will be further explained below with reference to the attached drawings and examples.
Attached drawing 1 is 10ppm benzoate and sorbate Surface enhanced Raman spectroscopy；
Attached drawing 2 is the detection of sorbate and benzoate in supernatant liquid sample；
Attached drawing 3 is the detection of sorbate and benzoate in troubled liquor sample；
Attached drawing 4 is the detection of sorbate and benzoate in solid sample；
Attached drawing 5 is the detection of mark-on sorbate and benzoate in fresh pork；
Attached drawing 6 is sorbate 1642cm in commercially available orange juice-1The linearity curve of intensity and concentration.
Specific embodiment
Nanogold synthesis: 100mL is first contained to 0.01% HAuCL4Solution is heated to boiling, and is rapidly added 1% lemon of 1mL
Lemon three sodium water solutions of acid, are heated to reflux 1h, are cooled to room temperature.
Nano silver synthesis: first the silver nitrate solution by 100mL containing 1mM is heated to boiling, and is rapidly added 1% citric acid of 1mL
Three sodium water solutions, are heated to reflux 1h, are cooled to room temperature.
Embodiment 1: taking 2mL supernatant liquid sample, commercially available amino acid, commercially available carbonated drink, commercially available cocktail, so-and-so commercially available energy
3mL methylene chloride, oscillation extraction is added in separatory funnel in beverage, and stratification takes 2mL supernatant in separatory funnel, adds
Enter 0.5mL aqueous solution 1mM sodium hydroxide, oscillation extraction.After stratification, lower layer's solution is taken out to be measured.Take 100 μ L to be measured
Liquid sequentially adds the sodium chloride that 100 μ L nanogold and 10uL concentration are 1M and mixes, be then placed on Raman spectrometer detection it is indoor into
Row detection.As a result see Fig. 2.
Embodiment 2: taking 5mL troubled liquor sample, and soy sauce (contains sorbate), and in separatory funnel, 0.5mL is added
10% trichloroacetic acid mixes centrifugation.It takes 4mL supernatant in separatory funnel, the acetic acid second of 0.5% acidifying with acetic acid of 5mL is added
Ester, oscillation extraction, stratification take 3mL supernatant in separatory funnel, and 1mL aqueous solution, oscillation extraction is added.Stratification
Afterwards, lower layer's solution is taken out to be measured.200 μ L prepare liquids are taken, the mixing of 100 μ L nanogold is sequentially added, is then placed on Raman spectrum
It is detected instrument detection interior.As a result see Fig. 3.
Embodiment 3: 1g is taken to shred solid sample, commercially available cake, commercially available preserved plum, commercially available hawthorn or commercially available preserved fruit, in beaker
In, the pentamethylene ultrasonic extraction of 1% acidifying with acetic acid of 5mL is added, takes 3mL supernatant in separatory funnel, 1mL concentration, which is added, is
0.01M sodium hydroxide, oscillation extraction.After stratification, lower layer's solution is taken out to be measured.50 μ L prepare liquids are taken, sequentially add 200
μ L nano silver mixes, and is then placed on Raman spectrometer detection interior and is detected.As a result see Fig. 4.
Embodiment 4: taking 2 parts of 2g slice fresh porks in beaker, be separately added into 50ppm sorbate and benzoate, then
The heptane ultrasonic extraction of 5% acidifying with acetic acid of 5mL is added, takes 3mL supernatant in separatory funnel, addition 1mL concentration is 0.1M hydrogen
Sodium oxide molybdena, oscillation extraction.After stratification, upper solution is transferred in another separatory funnel, 1mL secondary water, oscillation is added
Extraction, stratification.Lower layer's solution is taken out to be measured.100 μ L prepare liquids are taken, the mixing of 100 μ L nano silvers is sequentially added, then puts
It is detected in Raman spectrometer detection interior.As a result see Fig. 5.
Embodiment 6: taking five parts of commercially available juice samples of 5mL in separatory funnel, and sorbate standard items are added, make its concentration
Respectively 0,50ppm, 200ppm, 500ppm, 1000ppm, are added 5mL ethyl acetate, oscillation extraction, and stratification takes on 4mL
For clear liquid in separatory funnel, addition 0.5mL concentration is 0.01M sodium hydroxide, oscillation extraction.After stratification, by lower layer's solution
It takes out to be measured.100 μ L prepare liquids are taken, 200 μ L nano silvers and 10uL concentration is sequentially added and is mixed for the potassium chloride of 1M, is then placed on
It is detected Raman spectrometer detection interior.SERS characteristic peak at sorbate 1642cm-1 is mapped with concentration, is as a result seen
Fig. 6.
Claims (9)
1. the detection method of benzoate and sorbate, includes the following steps: in a kind of food
1) appropriate amount of sample is weighed, appropriate organic solvent is added and extracts, wherein the mass volume ratio model of solid sample and organic solvent
It encloses for 1:1~1:10g/mL, the mass volume ratio range of fluid sample and organic solvent is 1:0.5~1:10g/mL；It is organic molten
It is added organic acid in agent in advance, the volume ratio range of organic solvent and organic acid is 10:1~1000:1；After extracting solution is centrifuged
It is transferred in separatory funnel, appropriate aqueous solution is added, vibrate, stratification, lower layer's solution is spare as prepare liquid；
2) it takes appropriate prepare liquid in Raman sample bottle, appropriate metal-sol is added and mixes, add suitable inorganic salts flocculation
Agent mixes, and is then placed on Raman spectrometer detection interior and is detected.
2. the detection method of benzoate and sorbate in a kind of food according to claim 1, it is characterised in that: institute
Stating organic solvent is one of petroleum ether, n-hexane, hexamethylene, heptane, methylene chloride, ethyl acetate or its mixed liquor.
3. the detection method of benzoate and sorbate in a kind of food according to claim 1, it is characterised in that: institute
The organic acid stated is acetic acid.
4. the detection method of benzoate and sorbate in a kind of food according to claim 3, it is characterised in that: second
Acid concentration is 0.1%-10%.
5. the detection method of benzoate and sorbate in a kind of food according to claim 3, it is characterised in that: step
It is rapid 1) described in pH value of water solution be adjusted to 8-13.
6. the detection method of benzoate and sorbate in a kind of food according to claim 1, it is characterised in that: institute
Stating inorganic salts flocculant is at least one in sulfate, nitrate, carbonate, silicate, acetate, phosphate or halide salt
Kind.
7. the detection method of benzoate and sorbate in a kind of food according to claim 6, it is characterised in that: institute
State prepare liquid, metal-sol, inorganic salts flocculant additional amount be the 10 μ L:10 μ μ L:10 μ of L~500 of μ L~200 L of volume ratio~
500μL。
8. the detection method of benzoate and sorbate in a kind of food according to any one of claims 1 to 7,
Be characterized in that: step 1) or 2) before, further include standard curve preparation step, in food the benzoate of mark-on various concentration and
The feature peak intensity that spiked levels and scanning obtain is drawn standard curve by sorbate；Benzoate surface-enhanced Raman light
The characteristic peak of spectrum is 839cm-1, 1001cm-1, 1023cm-1Or 1597cm-1, the feature of sorbate Surface enhanced Raman spectroscopy
Peak is 1154cm-1, 1377cm-1Or 1642cm-1。
9. the detection method of benzoate and sorbate in a kind of food according to claim 8, it is characterised in that: also
Including step 3), the testing result of step 2) and the standard curve of drafting are compared, benzoate and sorbic acid in food are obtained
Salt quantitative analysis results.
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