CN102914606A - Qualitative and quantitative method for various biogenic amines in white wine - Google Patents
Qualitative and quantitative method for various biogenic amines in white wine Download PDFInfo
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Abstract
The invention discloses a qualitative and quantitative method for various biogenic amines in white wine and belongs to the technical field of white wine analysis and detection. According to the qualitative and quantitative method, the liquid-liquid extraction is utilized to enrich the biogenic amines in the white wine; derivation is required by both gas phase qualitative treatment and liquid phase quantitative treatment; a derivation agent adopted by the gas phase is TFAA (Trifluoroacetic Anhydride); and dansyl chloride precolumn derivatization is taken as the derivation agent for the liquid phase. According to the method provided by the invention, 9 biogenic amines are firstly determined in the white wine; the limit of detection of the quantitative method can be reduced to about 10ug/L; the linearly dependent coefficient is more than 0.99; the recovery rate is 80.19%-104.05%; the relative standard deviation is within 4%; the biogenic amines in the white wine can be detected by using the qualitative and quantitative method; the feasibility is excellent; and the precision is high.
Description
Technical field
The qualitative and quantitative method of multiple biogenic amine in the liquor, a kind of qualitative and quantitative method for biogenic amine in the liquor (nail amine, ethamine, pyrrolidine, putrescine, cadaverine) specifically, be specifically related to use gas chromatography-tandem mass spectrum coupling technique (GC-MS/MS) qualitative with ultraviolet detection-reversed-phase high-performance liquid chromatography technology (RP-HPLC) quantivative approach.The invention belongs to Liquor Analysis detection technique field.
Background technology
Up to the present, the biogenic amine in several large aromatic white spirits of China (biogenic amines is called for short BAs) research also belongs to blank, also the qualitative and quantitative method of not setting up for biogenic amine in the multiple aromatic white spirit of China.The biogenic amine kind that wherein exists and content thereof are unknown.
Biogenic amine is poisonous, the food that contains biogenic amine when the humans and animals excess intake, can cause poisoning, report in the world a lot of events of poisoning owing to the excess intake biogenic amine, secondary amine such as putrescine, cadaverine and pyrrolidine also can generate carcinogenic nitrosamine with the nitrite reaction.When the biogenic amine (taking in especially simultaneously multiple biogenic amine) of human body excess intake, can cause such as headache, feel sick, the allergic reactions such as palpitaition, blood pressure change, disordered breathing, the serious entail dangers to life of going back.Human body is taken in histamine and is reached 100mg when above, namely easily poisons.The histamine in the grape wine has been formulated clear and definite limit standard in the world, regulation content must not be higher than 10mg/L in Switzerland, and Germany, Belgium, French limit standard is lower, is respectively 2mg/L, 5 ~ 6mg/L, 8mg/L.
Many methods have been arranged for detection of the biogenic amine in the food, comprised thin-layered chromatography (TLC), vapor-phase chromatography (GC), capillary electrophoresis, high performance liquid chromatography (HPLC) etc.So far, all many about the research of biogenic amine in the fermented wine (grape wine, beer, yellow rice wine), the biogenic amine kind sum that detects in fermented wine reaches tens kinds more than.The detection of biogenic amine also still belongs to blank at present in the Spirit, and liquor will be studied biogenic amine wherein as one of the world's six large Spirits, top priority be first the biogenic amine kind in the liquor is carried out qualitative, and then quantitative.
Biogenic amine in the liquor is carried out when qualitative, at first be to concentrate biogenic amine in the liquor first, the concentrated general method that adopts can select to revolve steaming or nitrogen blows, and this sample size of testing qualitative employing is large, after selecting wine sample 375mL concentrated hydrochloric acid acidifying (pH 1.5), utilize Rotary Evaporators (40 ℃, vacuumize) to revolve and steam to 50mL.
All adopted liquid-liquid extraction in the qualitative, quantitative process, namely a kind of organic solvent or several organic mixed extractant solvent go out the biogenic amine in the sample, reach the purpose of purification, and remolding sensitivity is higher.The basic step of liquid-liquid extraction comprises: NaCl is saturated, then transfers to alkalescence, uses at last organic solvent (normal butyl alcohol-chloroform, normal butyl alcohol) extraction.PH can have influence on extraction efficiency, and research discovery pH is that the percentage extraction of 11.5 o'clock biogenic amines is the highest.
Summary of the invention
The objective of the invention is to set up the qualitative and quantitative method of multiple BAs in the liquor.Comprise the separation of biogenic amine, gas phase is derivative, liquid phase column front derivation condition is optimized and screens, and obtains qualitative, the quantitative method of biogenic amine in the complete liquor of a cover.This method has that to separate concentrated effect good, the advantage that the derivatization effect is high.
Technical scheme of the present invention: the qualitative and quantitative method of multiple biogenic amine BAs in a kind of liquor, use gas chromatography-tandem mass spectrum coupling technique GC-MS/MS qualitative quantitative with ultraviolet detection-reversed-phase high-performance liquid chromatography technology RP-HPLC, utilize the biogenic amine in the liquid-liquid extraction enrichment liquor, gas phase is qualitative quantitatively all to be needed to derive with liquid phase, the derivating agent that gas phase is selected is trifluoroacetic anhydride TFAA, the derivating agent that liquid phase adopts is the dansyl Cl column front derivation, comprise the separation of biogenic amine, gas phase is derivative, liquid phase column front derivation condition is optimized and screens;
(1) GC-MS quilitative method
Separate with derivative: after the 375mL wine sample concentrated hydrochloric acid acidifying (pH1.5), utilize Rotary Evaporators (40 ℃, vacuumize) to revolve and steam to 50mL, revolve and to add beaded glass when steaming and prevent bumping; Remaining liq revolves and steams 2 ~ 3 min with dichloromethane extraction twice, raffinate, transfers alkalescence (pH11), with 60mL butanols extraction three times.Solvent layer is washed with the NaOH of equal-volume 1M first, and then the HCl with two volumes 1M washes.The HCl elute soln again with the butanols extraction once.The residual salts acid solution is evaporated to dry salt.Dry salt is that 5mL trifluoroacetic anhydride (TFAA) is derivative with the derivating agent consumption, and derivatization reaction can not contain water, strictly seal, and 55 ℃, water-bath 30min; Then use the saturated NaHCO of 20mL
3Wash.Add solid NaHCO
3Until solution becomes is alkaline.Then use the 15mL extracted with diethyl ether.The diethyl ether solution saturated NaHCO of 20mL
3Wash, use again ultrapure washing.Adding anhydrous sodium sulfate drying spends the night.Nitrogen blows to 100uL, analyzes with GC-MS at once.
GC conditions: the chromatographic condition that FFAP post (60m * 0.25mm * 0.25 μ m) separates: gas chromatographic sample introduction mouth and detector temperature are 250 ℃, and carrier gas is helium, flow velocity 2mL/min; Sample size 1 μ L, Splitless injecting samples; The chromatographic column heating schedule: 50 ℃ of initial temperature, keep 2min, rise to 230 ℃ with 4 ℃/min, keep 15min.
Mass spectrum condition: EI ionization source; Electron energy: 70eV; Ion source temperature: 230 ℃; Sweep limit: 35 ~ 350amu.
(2) HPLC quantivative approach
Separate with derivative: the 5mL Wine Sample, adding 1.5g NaCl is saturated, adds 3mL normal butyl alcohol and chloroform (v/v 1:1) mixed extractant solvent, is 13 Na with pH
2CO
3Transfer pH to 11.5 with NaOH buffer solution, vortex instrument rotation concussion 4min collects organic phase, twice of re-extract.Add 1mL 1M HCl mixing, nitrogen dries up, and adds 2mL 0.1M HCl dissolving, add 2mL dansyl Cl derivating agent (9mg/mL, solvent are acetone), transferring pH is 8.6, the volumetric usage of derivating agent is identical with derivative front sample volume, behind the concussion mixing, and 40 ℃ of derivative 1h of water-bath lucifuges.Behind derivative the end, add 200 μ L ammoniacal liquor and interrupt reaction, add 3mL ethyl acetate, re-extract three times, combining extraction liquid, nitrogen dries up, and adds the dissolving of 1mL acetonitrile, the organic membrane filtration of 0.45 μ m, sample introduction.
Liquid phase chromatogram condition: Agilent C18 chromatographic column (4.6 * 250mm, 5 μ m), the detection wavelength is 254nm, and column temperature is 20 ℃, and sample size 10 μ L utilize the external standard method peak area quantification.Gradient elution, flow velocity are 0.4mL/min, and mobile phase A is acetonitrile, and B is ultrapure water.Elution program: 0 ~ 6min, A are 30%; 6 ~ 12min, A are 30% ~ 80%; 12 ~ 25min, A are 80% ~ 85%; 25 ~ 32min, A are 85% ~ 30%.
Beneficial effect of the present invention: the method that the present invention sets up is qualitative to 9 kinds of biogenic amines first in liquor, the quantivative approach detectability can be low to moderate about 10 μ g/L, linearly dependent coefficient is greater than 0.99, and the recovery is 80.19% ~ 104.05%, and relative standard deviation is in 4%.Illustrate that the biogenic amine in the liquor can utilize the method to detect, feasibility is good, and precision is high.
Description of drawings
Fig. 1 biogenic amine standard items GC-MS ion current chromatogram.
5 kinds of biogenic amine HPLC of Fig. 2 standard items chromatogram.1. methylamine, 2. ethamine, 3. pyrrolidine, 4. putrescine, 5. cadaverine.
The typical curve of Fig. 3 methylamine, ethamine, putrescine.
Fig. 4 pyrrolidine typical curve.
Fig. 5 cadaverine typical curve.
Embodiment
The qualitative, quantitative of biogenic amine in the embodiment 1 a certain commercially available liquor
After the 375mL wine sample concentrated hydrochloric acid acidifying (pH1.5), utilize Rotary Evaporators (40 ℃, vacuumize) to revolve and steam to 50mL, remaining liq revolves and steams 2 ~ 3 min with dichloromethane extraction twice, raffinate, transfers alkalescence (pH11), with 60mL butanols extraction three times.Solvent layer is washed with the NaOH of equal-volume 1M first, and then the HCl with two volumes 1M washes.HCl solution again with the butanols extraction once.The residual salts acid solution is evaporated to dry salt.Dry salt is derivative with 5mL trifluoroacetic anhydride (TFAA), then uses the saturated NaHCO of 20mL
3Wash.Add solid NaHCO
3Until solution becomes is alkaline.Then use the 15mL extracted with diethyl ether.The diethyl ether solution saturated NaHCO of 20mL
3Wash, use again ultrapure washing.Adding anhydrous sodium sulfate drying spends the night.Nitrogen blows to 100 μ L, analyzes with GC-MS at once.
Qualitative 9 kinds of biogenic amines that arrive and retention time in the table 1-a liquor
| Retention time min | Title | Biogenic amine TFAA derivant |
| 14.52 | Ethamine | Acetamide, N-ethyl-2,2,2-trifluoro- |
| 15.44 | Methylamine | Acetamide, 2,2,2-trifluoro-N-methyl- |
| 16.18 | Pyrrolidine | N-(Trifluoroacetyl)pyrrolidine |
| 17.97 | Isoamyl amine | Acetamide, 2,2,2-trifluoro-N-isopentyl- |
| 19.13 | Cyclopentamine | N-Cyclopentyl-trifluoroacetamide |
| 20.17 | Cyclohexylamine | Acetamide, N-cyclohexyl-2,2,2-trifluoro- |
| 22.62 | Cycloheptylamine | Trifluoroacetamide, N-cycloheptyl |
| 36.71 | Putrescine | 2,2,2-Trifluoro-N-[4-(2,2,2-trifluoro-acetylamino)-butyl]-acetamide |
| 37.86 | Cadaverine | 2,2,2-Trifluoro-N-[4-(2,2,2-trifluoro-acetylamino)-amyl]-acetamide |
The qualitative biogenic amine kind that arrives in the table 1-b one commercially available liquor
| Retention time min | Title | Biogenic amine TFAA derivant |
| 14.52 | Ethamine | Acetamide, N-ethyl-2,2,2-trifluoro- |
| 15.44 | Methylamine | Acetamide, 2,2,2-trifluoro-N-methyl- |
| 16.18 | Pyrrolidine | N-(Trifluoroacetyl)pyrrolidine |
| 36.71 | Putrescine | 2,2,2-Trifluoro-N-[4-(2,2,2-trifluoro-acetylamino)-butyl]-acetamide |
| 37.86 | Cadaverine | 2,2,2-Trifluoro-N-[4-(2,2,2-trifluoro-acetylamino)-amyl]-acetamide |
Draw wine sample 5mL, adding 1.5g NaCl is saturated, adds 3mL normal butyl alcohol and chloroform (1:1) mixed extractant solvent, is 13 Na with pH
2CO
3Transfer pH to 11.5 with NaOH buffer solution, vortex instrument rotation concussion 4min collects organic phase, twice of re-extract.Add 1mL 1MHCl mixing, nitrogen dries up, and adds 2mL 0.1M HCl dissolving, adds 2mL dansyl Cl derivating agent (9mg/mL, solvent are acetone), and transferring pH is 8.6, behind the concussion mixing, and 40 ℃ of derivative 1h of water-bath lucifuge.Behind derivative the end, add 200 μ L ammoniacal liquor and interrupt reaction, add 3mL ethyl acetate, re-extract three times, combining extraction liquid, nitrogen dries up, and adds the dissolving of 1mL acetonitrile, the organic membrane filtration of 0.45 μ m, sample introduction.Record its EC content and see Table 2.
Content of Biogenic Amines (μ g/L) in the table 2 commercially available liquor
| The wine sample | Methylamine | Ethamine | Pyrrolidine | Putrescine | Cadaverine | Total amount |
| Liquor | 15.47 | 35.56 | 1418.88 | 91.83 | ql | 1561.74 |
The recovery, precision and the detectability of test example HPLC method detection of biological amine
1, column front derivation
(1) preparation of dansyl Cl solution: take by weighing in the acetone that the 90mg dansyl Cl is dissolved in 10mL, keep in Dark Place.
(2) derivative step: same Wine Sample mark-on is derivative, adds 2mL dansyl Cl derivating agent (9mg/mL, solvent are acetone), and transferring pH is 8.6, behind the concussion mixing, and 40 ℃ of derivative 1h of water-bath lucifuge.After reaction finishes, add 3mL ethyl acetate, re-extract three times, combining extraction liquid, nitrogen dries up, and adds the dissolving of 1mL acetonitrile, and the organic membrane filtration of 0.45 μ m is used for analyzing and testing.
2, high performance liquid chromatography (HPLC) standard measure biogenic amine
Adopt Agilent C18 chromatographic column (4.6 * 250mm, 5 μ m), mobile phase adopts acetonitrile and water, carries out gradient elution (seeing Table 3), and the gradient elution program sees the following form, and flow velocity is 0.4mL/min, and column temperature is 20 ℃, and the detection wavelength is 254nm.
Table 3 gradient elution program
| Elution time (min) | Mobile phase A (%) | Mobile phase B (%) |
| 0-6 | 30 | 70 |
| 6-12 | 30-80 | 70-20 |
| 12-25 | 80-85 | 20-15 |
| 25-32 | 85-30 | 15-70 |
The range of linearity of method
With the HCl of 0.1M as solvent, respectively to the standard reserving solution for the treatment of 5 kinds of quantitative biogenic amines that wherein adds each suitable concn, become 10 concentration gradients by the concentration stepwise dilution that reduces by half, derive according to the disposal route of sample, RP-HPLC analyzes, drawing standard curve (seeing Table 4).
5 kinds of biogenic amine regression equations of table 4 and related coefficient
| Biogenic amine | The range of linearity (mg/L) | Curvilinear equation | R 2 |
| Methylamine | 0.014~1.87 | y=0.0173x+0.027 | 0.9936 |
| Ethamine | 0.020~2.66 | y=0.034x-0.0092 | 0.9966 |
| Pyrrolidine | 0.095~12.17 | y=0.0727x-4.371 | 0.9911 |
| Putrescine | 0.014~1.89 | y=0.0288x+0.0328 | 0.9964 |
| Cadaverine | 0.016~4.14 | y=0.0291x-0.0831 | 0.9914 |
Recovery precision and the detection limit of method
Same Wine Sample mark-on is carried out quantitatively (n=5), sample introduction respectively, calculate recovery rate calculates the relative standard deviation (RSD) (seeing Table 5) of the method simultaneously by replica test.
The detectability of table 5 method and the recovery
| Biogenic amine | Relative standard deviation (%) | Detectability (mg/L) | The recovery (%) |
| Methylamine | 2.95 | 0.013 | 97.35 |
| Ethamine | 2.88 | 0.008 | 104.05 |
| Pyrrolidine | 3.25 | 0.032 | 80.19 |
| Putrescine | 2.21 | 0.002 | 87.84 |
| Cadaverine | 2.68 | 0.001 | 99.89 |
Detection limit: signal to noise ratio (S/N ratio) is 3.
Claims (1)
1. the qualitative and quantitative method of multiple biogenic amine BAs in the liquor, it is characterized in that using gas chromatography-tandem mass spectrum coupling technique GC-MS/MS qualitative quantitative with ultraviolet detection-reversed-phase high-performance liquid chromatography technology RP-HPLC, utilize the biogenic amine in the liquid-liquid extraction enrichment liquor, gas phase is qualitative quantitatively all to be needed to derive with liquid phase, the derivating agent that gas phase is selected is trifluoroacetic anhydride TFAA, the derivating agent that liquid phase adopts is the dansyl Cl column front derivation, comprise the separation of biogenic amine, gas phase is derivative, liquid phase column front derivation condition is optimized and screens;
(1) GC-MS quilitative method
Separation and derivative: pH 1.5 is transferred in the acidifying of 375mL wine sample concentrated hydrochloric acid, utilizes 40 ℃ of Rotary Evaporators, vacuumizes to revolve to steam and arrive 50mL, will add beaded glass when revolving steaming and prevent bumping; Remaining liq revolves and steams 2 ~ 3min with dichloromethane extraction twice, raffinate, transfers alkaline pH 11, with 60mL butanols extraction three times; Solvent layer is washed with the NaOH of equal-volume 1M first, and then the HCl with two volumes 1M washes, and the HCl elute soln again with the butanols extraction once remains the HCl solution decompression and is concentrated into dry salt; Dry salt is that 5mL trifluoroacetic anhydride TFAA is derivative with the derivating agent consumption, and derivatization reaction can not contain water, strictly seal, and 55 ℃, water-bath 30min; Then use the saturated NaHCO of 20mL
3Wash, add solid NaHCO
3Until solution becomes is alkaline, then use the 15mL extracted with diethyl ether, the diethyl ether solution saturated NaHCO of 20mL
3Wash, use ultrapure washing again, add anhydrous sodium sulfate drying and spend the night, nitrogen blows to 100 μ L, analyzes with GC-MS at once;
GC conditions: the chromatographic condition that FFAP post 60m * 0.25mm * 0.25 μ m separates: gas chromatographic sample introduction mouth and detector temperature are 250 ℃, and carrier gas is helium, flow velocity 2mL/min; Sample size 1 μ L, Splitless injecting samples; The chromatographic column heating schedule: 50 ℃ of initial temperature, keep 2min, rise to 230 ℃ with 4 ℃/min, keep 15min;
Mass spectrum condition: EI ionization source; Electron energy: 70eV; Ion source temperature: 230 ℃; Sweep limit: 35 ~ 350amu;
(2) HPLC quantivative approach
Separate with derivative: the 5mL Wine Sample, adding 1.5g NaCl is saturated, adds the 3mL normal butyl alcohol: the mixed extractant solvent of chloroform volume ratio 1:1, with the Na of pH 13
2CO
3Transfer pH to 11.5 with NaOH buffer solution, vortex instrument rotation concussion 4min collects organic phase, twice of re-extract; Add 1mL 1M HCl mixing, nitrogen dries up, and adds 2mL 0.1M HCl dissolving, adding 2mL dansyl Cl 9mg/mL, solvent are the dansyl Cl derivating agent of acetone, and transferring pH is 8.6, and the volumetric usage of derivating agent is identical with derivative front sample volume, behind the concussion mixing, 40 ℃ of derivative 1h of water-bath lucifuge; Behind derivative the end, add 200 μ L ammoniacal liquor and interrupt reaction, add 3mL ethyl acetate, re-extract three times, combining extraction liquid, nitrogen dries up, and adds the dissolving of 1mL acetonitrile, the organic membrane filtration of 0.45 μ m, sample introduction;
Liquid phase chromatogram condition: Agilent C18 chromatographic column 4.6 * 250mm, 5 μ m, the detection wavelength is 254nm, column temperature is 20 ℃, and sample size 10 μ L utilize the external standard method peak area quantification, gradient elution, flow velocity is 0.4mL/min, and mobile phase A is acetonitrile, and B is ultrapure water, elution program: 0 ~ 6min, A are 30%; 6 ~ 12min, A are 30% ~ 80%; 12 ~ 25min, A are 80% ~ 85%; 25 ~ 32min, A are 85% ~ 30%.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106770716A (en) * | 2016-11-28 | 2017-05-31 | 无锡艾科瑞思产品设计与研究有限公司 | Histamine detection method and kit in a kind of animal tissue |
| CN108872414A (en) * | 2018-04-24 | 2018-11-23 | 许昌学院 | A kind of method that LC-MS/MS measures the cadaverine in soy sauce |
| CN109725095A (en) * | 2019-01-22 | 2019-05-07 | 灏博农业科技(杭州)有限公司 | A method of a variety of Content of Biogenic Amines in soy sauce are detected using HPLC simultaneously |
| CN110850005A (en) * | 2019-12-19 | 2020-02-28 | 常州磐诺仪器有限公司 | Method for rapidly detecting histamine content in fruit wine |
| CN111879860A (en) * | 2019-11-27 | 2020-11-03 | 江南大学 | Method for accurately detecting content of pentamethylene diamine in fermentation liquor |
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-
2012
- 2012-10-20 CN CN201210400028.5A patent/CN102914606B/en active Active
Non-Patent Citations (12)
| Title |
|---|
| 《Analytica Chimica Acta》 20061107 Silvia Millan et al. Simple and rapid determination of biogenic amines in wine by liquid chromatography-electrospray ionization ion trap mass spectrometry 145-152 1 , * |
| O. BUSTO ET AL.: "Determination of biogenic amines in wine after precolumn derivatization with 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate", 《JOURNAL OF CHROMATOGRAPHY A》 * |
| R. ROMERO ET AL.: "Optimization of chromatographic parameters for the determination of biogenic amines in wines by reversed-phase high-performance liquid chromatography", 《JOURNAL OF CHROMATOGRAPHY A》 * |
| SILVIA MILLAN ET AL.: "Simple and rapid determination of biogenic amines in wine by liquid chromatography–electrospray ionization ion trap mass spectrometry", 《ANALYTICA CHIMICA ACTA》 * |
| 文萃: "邻苯二醛柱前自动衍生-反向高效液相色谱法测定食物中的生物胺 ", 《国外医学(卫生学分册)》 * |
| 文萃: "邻苯二醛柱前自动衍生-反向高效液相色谱法测定食物中的生物胺", 《国外医学(卫生学分册)》, vol. 23, no. 04, 31 July 1996 (1996-07-31), pages 243 - 244 * |
| 李志军等: "葡萄酒中生物胺多组分的UVD/FLD串联HPLC方法研究 ", 《卫生研究》 * |
| 李志军等: "葡萄酒中生物胺多组分的UVD/FLD串联HPLC方法研究", 《卫生研究》, vol. 34, no. 05, 30 September 2005 (2005-09-30), pages 577 - 580 * |
| 谢铭: "黄酒中生物胺的分析研究 ", 《广州化工》 * |
| 谢铭: "黄酒中生物胺的分析研究", 《广州化工》, vol. 38, no. 04, 31 December 2010 (2010-12-31), pages 139 - 141 * |
| 陆永梅等: "高效液相色谱法测定黄酒中生物胺的含量 ", 《食品科学》 * |
| 陆永梅等: "高效液相色谱法测定黄酒中生物胺的含量", 《食品科学》, vol. 27, no. 01, 31 January 2006 (2006-01-31), pages 196 - 199 * |
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| CN106770716A (en) * | 2016-11-28 | 2017-05-31 | 无锡艾科瑞思产品设计与研究有限公司 | Histamine detection method and kit in a kind of animal tissue |
| CN108872414A (en) * | 2018-04-24 | 2018-11-23 | 许昌学院 | A kind of method that LC-MS/MS measures the cadaverine in soy sauce |
| CN109725095A (en) * | 2019-01-22 | 2019-05-07 | 灏博农业科技(杭州)有限公司 | A method of a variety of Content of Biogenic Amines in soy sauce are detected using HPLC simultaneously |
| CN111879860A (en) * | 2019-11-27 | 2020-11-03 | 江南大学 | Method for accurately detecting content of pentamethylene diamine in fermentation liquor |
| CN111879860B (en) * | 2019-11-27 | 2021-09-28 | 江南大学 | Method for accurately detecting content of pentamethylene diamine in fermentation liquor |
| CN112903886A (en) * | 2019-12-04 | 2021-06-04 | 四川科伦药物研究院有限公司 | Separation and detection method of 1-butylsulfonyl chloride related substances |
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| CN110850005A (en) * | 2019-12-19 | 2020-02-28 | 常州磐诺仪器有限公司 | Method for rapidly detecting histamine content in fruit wine |
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