CN104297359B - A kind of method of seven kinds of composition Simultaneously test in flavoring essence spices - Google Patents
A kind of method of seven kinds of composition Simultaneously test in flavoring essence spices Download PDFInfo
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Abstract
The invention discloses the method for seven kinds of composition Simultaneously test in a kind of flavoring essence spices, comprise the following steps: the calculating of the preparation of the preparation of extraction solution, the preparation of standard solution, sample solution, Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry Analysis and content.The present invention is by the optimization of the Pretreatment to seven kinds of method for measuring components in flavoring essence spices, liquid phase chromatogram condition and Mass Spectrometry Conditions, establish a kind of easy, quick, high-throughout assay method, the present invention have simple to operate, highly sensitive, the recovery is good, favorable reproducibility and detection time is short, solvent consumption is little, detect the advantage that flux is high, detection efficiency is high.
Description
Technical field
The invention belongs to physical and chemical inspection technical field, to be specifically related in a kind of flavoring essence spices the method for seven kinds of composition salicylic acids, sodium cyclohexylsulfamate, benzoic acid, methyl p-hydroxybenzoate, ethyl ester, propyl ester, butyl ester Simultaneously test.
Background technology
Salicylic acid has another name called septichen, it is important fine chemical material, in medical industry, salicylic acid is a very wide range of sterilization of a kind of purposes, antiseptic, salicylic acid is all classified as and limits the use of adjuvant by many countries, forbid for food processing and production at China's salicylic acid, China GB GB7916-1987 specifies that its highest safe level massfraction is 0.15%.Salicylic acid is organic acid antiseptic, has stronger antimycotic character in acid condition, and toxicology test research shows, preservative ingredient consumption too much can produce harm to human liver, even carcinogenic.FDA (Food and Drug Adminstration), skin disease association of the U.S. think that salicylic threshold limit values is 0.5%-2.0%.Report that measuring salicylic detection method has photometry, vapor-phase chromatography, liquid phase chromatography etc. at present.
Benzoic acid is antiseptic conventional in food industry, effectively can prevent the growth of yeast, mould, bacterium, but excessive, long-term edible meeting harmful to human liver, renal function.The benzoic maximum use limitation of clear stipulaties in standard GB/T 2760-2007.In foreign trade, the states such as Japan require that the detected level of this material is less than 1mg/kg, and in China standard GB/T23495-2009, benzoic acid is 1.8mg/kg, and in GB/T5009.29-2003, benzoic detection limit is 1mg/kg.Report that measuring benzoic detection method has gas chromatography-mass spectrography, high performance liquid chromatography etc. at present.
P-hydroxybenzoate (also known as nipagin esters), the sterilizing ability good because of it and stability, be widely used in the numerous areas such as food, beverage, cosmetics, mainly as antiseptic.Nipagin esters comprises methyl esters, ethyl ester, propyl ester, butyl ester etc., and its bacteriostasis increases along with the increase of alcohol alkyl carbon number, and carbochain is longer, and toxicity is less, and consumption is fewer.In production run, normally by used in combination for several ester, while raising solubleness, there is better antiseptic property.Practical applications a large amount of both at home and abroad also demonstrate that mixed nipagin esters is stronger than single fungistatic effect.Though nipagin esters has good antisepsis, also there is certain toxicity.Many countries and the international organization uses to Determination of p-hydroxybenzoate Antiseptics in Foods such as China, Canada, Japan and European Union have been formulated and have been added limitation.The Late Cambrian p-hydroxybenzoates such as Routledge have estrogen active, and its excessive use can be detrimental to health.The use standard GB2760-2011 of Food Additives Used in China defines single variety and maximum use amount used in combination, and wherein propylparaben is clearly prohibitted the use, and butyl p-hydroxybenzoate is not put into permission yet and uses list.The assay method of nipagin esters mainly contains high performance liquid chromatography, thin-layered chromatography, vapor-phase chromatography, gas chromatography-mass spectrography etc.
Honey element, chemistry sodium cyclohexylsulfamate by name is a kind of artificial synthesis edulcorant low in calories, it is Prof. Du Yucang non-nutritive sweeteners conventional in food production, its sugariness is sucrose 30-40 times, and use cost is low, therefore extensively adds in the food such as beverage, cake, preserved fruit.In recent years, Determination of Saccharin in Food content overproof and forbidding that adding the report adding honey element in the food of honey element day by day increases, therefore, honey element is excessive edible, will work the mischief to the liver of human body and nervous system because of excess intake, particularly more obvious to the more weak old man of the ability of metabolism, pregnant woman, child's harm.The assay method of honey element mainly contains By Gas Chromatography-mass Spectrometry, the chromatography of ions, Liquid Chromatography-Tandem Mass Spectrometry etc.
At present, domestic and international open source literature has nothing to do the method simultaneously detected in this seven kinds of compositions.
Summary of the invention
To the object of the present invention is to provide in a kind of flavoring essence spices the method for seven kinds of composition salicylic acids, sodium cyclohexylsulfamate, benzoic acid, methyl p-hydroxybenzoate, ethyl ester, propyl ester, butyl ester Simultaneously test.
The present invention is directed to the deficiencies in the prior art, by long-term research and exploration, the basis of method contrast, optimization proposes the method for seven kinds of composition (salicylic acid, sodium cyclohexylsulfamate, benzoic acid, methyl p-hydroxybenzoate, ethyl ester, propyl ester, butyl ester) Simultaneously test in a kind of flavoring essence spices, for detecting salicylic acid, sodium cyclohexylsulfamate, benzoic acid, methyl p-hydroxybenzoate, ethyl ester, propyl ester, the butyl ester in flavoring essence spices.The present invention has investigated the Pretreatment of salicylic acid, sodium cyclohexylsulfamate, benzoic acid, methyl p-hydroxybenzoate, ethyl ester, propyl ester, butyl ester in flavoring essence spices, liquid phase chromatogram condition and Mass Spectrometry Conditions, for seven kinds of compositions in easy, quick, high-throughout mensuration flavoring essence spices provide technical support.
Technical scheme of the present invention is: described assay method comprises the following steps:
The preparation of A, extraction solution: the methanol-water solution getting Methanol standby one-tenth volume ratio 7:3 is extraction solution;
The preparation of B, standard solution: with the standard solution preparing salicylic acid, sodium cyclohexylsulfamate, benzoic acid, methyl p-hydroxybenzoate, ethyl ester, propyl ester, butyl ester containing interior target extraction solution respectively;
The preparation of C, sample solution: use containing interior target extraction solution extraction flavoring essence fragrance sample, obtain sample solution after crossing organic phase filter membrane;
D, Ultra Performance Liquid Chromatography-tandem mass spectrometer analysis: utilize Ultra Performance Liquid Chromatography-tandem mass spectrometer to carry out detection to standard solution and sample solution respectively and analyze;
The calculating of seven kinds of composition salicylic acids, sodium cyclohexylsulfamate, benzoic acid, methyl p-hydroxybenzoate, ethyl ester, propyl ester, butyl ester content in E, flavoring essence spices.
The preparation of standard solution described in step B is: take salicylic acid, sodium cyclohexylsulfamate, benzoic acid, methyl p-hydroxybenzoate, ethyl ester, propyl ester, each 20mg of butyl ester respectively, be transferred in the brown volumetric flask of 100mL after dissolving with methyl alcohol, be settled to scale, obtain single standard storing solution respectively; Take salicylic acid-d410mg, be transferred in the brown volumetric flask of 50mL after dissolving with methyl alcohol, methanol constant volume, to scale, obtains interior mark storing solution; Get respectively in the brown volumetric flask of single standard storing solution 0.5 ~ 2mL to 50mL, by methanol constant volume to scale, obtain one-level mixed standard solution; Get in the brown volumetric flask of interior mark storing solution 1mL to 50mL, by methanol constant volume to scale, obtain mark standard solution in one-level; Accurately pipette the one-level mixed standard solution of 0.1mL, 0.5mL, 1mL, 2mL, 5mL respectively in the brown volumetric flask of 50mL, each brown volumetric flask all adds mark standard solution in 1mL one-level, is settled to scale, obtains series standard solution with extraction solution.
Get mark storing solution in 0.4mL and, in the brown volumetric flask of 1L, be settled to scale with extraction solution, obtain containing interior target extraction solution.Described is salicylic acid-d4 containing the internal standard compound in interior target extraction solution.
The preparation method of sample solution described in step C is: take 0.5g sample in 50mL tool plug conical flask, and accurately add 25mL containing interior target extraction solution, with 150r/min oscillation extraction 20min, get supernatant and cross organic phase filter membrane, filtrate is sample solution.Described organic phase filter membrane is 0.22 μm of polyethersulfone membranes.The oscillation frequency of described oscillation extraction is 120-180r/min, and extraction time is 10-30min.
Chromatographiccondition described in D step is: chromatographic column: C18,1.7 μm, 2.1 × 100mm post; Mobile phase is methyl alcohol A and 0.05% aqueous formic acid B; Flow velocity: 0.4mL/min; Sample size: 5 μ L; Column temperature: 40 DEG C; Sample temperature: 10 DEG C; Adopt gradient elution program, namely initial A is 10%, B, and A is 35%, B when being 90%, 1min is 65%, during 4min, A is 65%, B, and initial A is 90%, B when being 35%, 6min when being 10%, 7min that A is 90%, when B is 10%, 8min, A is 10%, B, and A is 10%, B when being 90%, 10min is 90%.Described Mass Spectrometry Conditions is: electric spray ion source (ESI) negative ion mode, and scan mode is multiple-reaction monitoring pattern, and electron spray voltage is-4500V, ion source temperature 600 DEG C, gas curtain gas: 25Psi; Atomization gas: 55Psi; Auxiliary heating gas: 50Psi; The quota ion of salicylic acid, sodium cyclohexylsulfamate, benzoic acid, methyl p-hydroxybenzoate, ethyl ester, propyl ester, butyl ester and salicylic acid-d4 is to being respectively: m/z92.9,79.9,77.0,92.0,91.9,92.0,92.1,96.9.Other mass spectrometry parameters is in table 1.
The calculating of content described in E step is: first carry out regretional analysis with the chromatographic peak area of the object detected by standard solution and internal standard compound than its respective concentration ratio corresponding and obtain typical curve linear equation, the chromatographic peak area of the object then sample solution detected, substitute into typical curve linear equation, namely obtain the content of salicylic acid in sample, sodium cyclohexylsulfamate, benzoic acid, methyl p-hydroxybenzoate, ethyl ester, propyl ester, butyl ester.
The present invention is directed to the deficiencies in the prior art, by the optimization of the Pretreatment to salicylic acid, sodium cyclohexylsulfamate, benzoic acid, methyl p-hydroxybenzoate, ethyl ester, propyl ester, butyl ester in flavoring essence spices, chromatographic condition and Mass Spectrometry Conditions, establish a kind of easy, quick, high-throughout assay method, for the detection of kind of the composition of seven in flavoring essence spices provides technical support.The present invention have simple to operate, highly sensitive, the recovery is good, favorable reproducibility and detection time is short, solvent consumption is little, detect that flux is high, advantage that detection efficiency is high, the quality safety for supervision flavoring essence spices has very important significance.
Accompanying drawing explanation
Fig. 1 is the process flow diagram of assay method of the present invention.
Fig. 2 is salicylic typical curve linear equation and linear regression coeffficient coordinate diagram.
Fig. 3 is typical curve linear equation and the linear regression coeffficient coordinate diagram of sodium cyclohexylsulfamate.
Fig. 4 is benzoic typical curve linear equation and linear regression coeffficient coordinate diagram.
Fig. 5 is typical curve linear equation and the linear regression coeffficient coordinate diagram of methyl p-hydroxybenzoate.
Fig. 6 is typical curve linear equation and the linear regression coeffficient coordinate diagram of ethyl-para-hydroxybenzoate.
Fig. 7 is typical curve linear equation and the linear regression coeffficient coordinate diagram of propylparaben.
Fig. 8 is typical curve linear equation and the linear regression coeffficient coordinate diagram of butyl p-hydroxybenzoate.
Fig. 9 is the chromatogram of salicylic acid, sodium cyclohexylsulfamate, benzoic acid, methyl p-hydroxybenzoate, ethyl ester, propyl ester, butyl ester in standard solution.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is further illustrated, but limited the present invention never in any form, and any conversion done based on training centre of the present invention or replacement, all belong to protection scope of the present invention.
Embodiment 1:
The method of seven kinds of composition Simultaneously test in flavoring essence spices of the present invention, comprises the following steps:
(1) preparation of extraction solution: the methanol-water solution getting Methanol standby one-tenth volume ratio 7:3 is extraction solution;
(2) preparation of standard solution: with the standard solution preparing salicylic acid, sodium cyclohexylsulfamate, benzoic acid, methyl p-hydroxybenzoate, ethyl ester, propyl ester, butyl ester containing interior target extraction solution respectively;
(3) preparation of sample solution: use containing interior target extraction solution extraction flavoring essence fragrance sample, obtain sample solution after crossing organic phase filter membrane;
(4) Ultra Performance Liquid Chromatography-tandem mass spectrometer analysis: utilize Ultra Performance Liquid Chromatography-tandem mass spectrometer to carry out detection to standard solution and sample solution respectively and analyze;
(5) calculating of seven kinds of composition salicylic acids, sodium cyclohexylsulfamate, benzoic acid, methyl p-hydroxybenzoate, ethyl ester, propyl ester, butyl ester content in flavoring essence spices.
The preparation of standard solution described in step B is: take salicylic acid, sodium cyclohexylsulfamate, benzoic acid, methyl p-hydroxybenzoate, ethyl ester, propyl ester, each 20mg of butyl ester respectively, be transferred in the brown volumetric flask of 100mL after dissolving with methyl alcohol, be settled to scale, obtain single standard storing solution respectively; Take salicylic acid-d410mg, be transferred in the brown volumetric flask of 50mL after dissolving with methyl alcohol, methanol constant volume, to scale, obtains interior mark storing solution; Get respectively in the brown volumetric flask of single standard storing solution 0.5 ~ 2mL to 50mL, by methanol constant volume to scale, obtain one-level mixed standard solution; Get in the brown volumetric flask of interior mark storing solution 1mL to 50mL, by methanol constant volume to scale, obtain mark standard solution in one-level; Accurately pipette the one-level mixed standard solution of 0.1mL, 0.5mL, 1mL, 2mL, 5mL respectively in the brown volumetric flask of 50mL, each brown volumetric flask all adds mark standard solution in 1mL one-level, is settled to scale, obtains series standard solution with extraction solution.The described single standard storing solution 0.5mL-2mL that gets respectively is specially and gets salicylic acid, sodium cyclohexylsulfamate, methyl p-hydroxybenzoate, ethyl ester, propyl ester, butyl ester single standard storing solution 0.5mL respectively and get benzoic acid single standard storing solution 2mL.
Get mark storing solution in 0.4mL and, in the brown volumetric flask of 1L, be settled to scale with extraction solution, obtain containing interior target extraction solution.Described is salicylic acid-d4 containing the internal standard compound in interior target extraction solution.
The preparation method of sample solution described in step C is: take 0.5g sample in 50mL tool plug conical flask, and accurately add 25mL containing interior target extraction solution, with 150r/min oscillation extraction 20min, get supernatant and cross organic phase filter membrane, filtrate is sample solution.Sample solution Ultra Performance Liquid Chromatography-tandem mass spectrometer is analyzed.
Described organic phase filter membrane is 0.22 μm of polyethersulfone membranes.Liquid-phase chromatographic analysis condition described in D step is: chromatographic column: C18,1.7 μm, 2.1 × 100mm post; Mobile phase is methyl alcohol A and 0.05% aqueous formic acid B; Flow velocity: 0.4mL/min; Sample size: 5 μ L; Column temperature: 40 DEG C; Sample temperature: 10 DEG C; Adopt gradient elution program, namely initial A is 10%, B, and A is 35%, B when being 90%, 1min is 65%, during 4min, A is 65%, B, and initial A is 90%, B when being 35%, 6min when being 10%, 7min that A is 90%, when B is 10%, 8min, A is 10%, B, and A is 10%, B when being 90%, 10min is 90%.Described Mass Spectrometry Conditions is: electric spray ion source (ESI) negative ion mode, and scan mode is multiple-reaction monitoring pattern, and electron spray voltage is-4500V, ion source temperature 600 DEG C, gas curtain gas: 25Psi; Atomization gas: 55Psi; Auxiliary heating gas: 50Psi; The quota ion of salicylic acid, sodium cyclohexylsulfamate, benzoic acid, methyl p-hydroxybenzoate, ethyl ester, propyl ester, butyl ester and salicylic acid-d4 is to being respectively: m/z92.9,79.9,77.0,92.0,91.9,92.0,92.1,96.9.Other mass spectrometry parameters is in table 1.
The mass spectrometry parameters table of seven kinds of compositions in table 1 flavoring essence spices
The calculating of content described in E step is: first carry out regretional analysis with the chromatographic peak area of the object detected by standard solution and internal standard compound than its respective concentration ratio corresponding and obtain typical curve linear equation, the chromatographic peak area of the object then sample solution detected, substitute into typical curve linear equation, namely obtain the content of salicylic acid in sample, sodium cyclohexylsulfamate, benzoic acid, methyl p-hydroxybenzoate, ethyl ester, propyl ester, butyl ester.
The regression equation corresponding with typical curve, related coefficient etc. are as shown in table 2.
The typical curve equation of seven kinds of compositions and detection limit in table 2 flavoring essence spices
Then the chromatographic peak area detecting object sample recorded, substitute into typical curve linear equation, namely obtain the concentration of salicylic acid in sample, sodium cyclohexylsulfamate, benzoic acid, methyl p-hydroxybenzoate, ethyl ester, propyl ester, butyl ester, calculate the content of salicylic acid, sodium cyclohexylsulfamate, benzoic acid, methyl p-hydroxybenzoate, ethyl ester, propyl ester, butyl ester in flavoring essence spices thus.
In flavoring essence fragrance sample, the cubage formula of seven kinds of compositions is as follows:
（1）
In formula:
X
ithe content of seven kinds of compositions in-sample, unit is milligrams per kilogram (mg/kg);
C
ithe concentration of seven kinds of compositions in the-sample that drawn by standard working curve, unit is milligrams per liter (mg/L);
C
i0the concentration of seven kinds of compositions in the-blank that drawn by standard working curve, unit is milligrams per liter (mg/L);
V-extraction solution volume, unit is milliliter (mL);
M-sample mass, unit is gram (g).
To the precision of the inventive method and the detection method of recovery of standard addition as follows: adopt sample carry out recovery of standard addition test, the standard solution adding basic, normal, high three variable concentrations levels respectively in the sample carries out recovery of standard addition test, each sample parallel measures 6 times, analysis condition is with embodiment 1, then calculate the relative standard deviation of measured value after the recovery of standard addition of seven kinds of compositions in this method flavoring essence spices and mark-on, the results are shown in Table 3.
The precision of seven kinds of compositions and the recovery (n=6) in table 3 flavoring essence spices
As can be seen from Table 3, under three mark-on levels, the average recovery rate of the seven kinds of compositions adopting the method to measure in flavoring essence spices is respectively: 93.59%, 92.78%, 92.49%, 96.64%, 96.89%, 101.34%, 97.74%, the relative standard deviation of sample determination result is respectively: 3.14%, 4.16%, 3.10%, 3.10%, 3.42%, 2.72%, 3.13%, explanation the method is stablized, the recovery of method is good, and precision is good.
The present invention examines repeatability, the repeatability and universality etc. of method by experiment, determine the Ultra Performance Liquid Chromatography-tandem mass spectrum detection method of salicylic acid in flavoring essence spices, sodium cyclohexylsulfamate, benzoic acid, methyl p-hydroxybenzoate, ethyl ester, propyl ester, butyl ester, reach following effect:
(1) detection time is short: adopt the present invention to measure the content cycle only 10min of salicylic acid, sodium cyclohexylsulfamate, benzoic acid, methyl p-hydroxybenzoate, ethyl ester, propyl ester, butyl ester in flavoring essence spices.
(2) solvent consumption is little.
(3) detect flux high, detection efficiency is high.
(4) the present invention has simple to operate, highly sensitive, good and the high repeatability and other advantages of the recovery, seven kinds of compositions all have good linear relationship, the detection limit of the method is between 0.008-0.023mg/kg, average recovery rate is respectively: 93.59%, 92.78%, 92.49%, 96.64%, 96.89%, 101.34%, 97.74%, and average relative standard's deviation of sample tests is: 3.14%, 4.16%, 3.10%, 3.10%, 3.42%, 2.72%, 3.13%.
(5) foundation of the method has very important significance for the quality safety of supervising flavoring essence spices.
Claims (7)
1. the method for seven kinds of composition Simultaneously test in flavoring essence spices, is characterized in that comprising the following steps:
The preparation of A, extraction solution: the methanol-water solution getting Methanol standby one-tenth volume ratio 7:3 is extraction solution;
The preparation of B, standard solution: with the standard solution preparing salicylic acid, sodium cyclohexylsulfamate, benzoic acid, methyl p-hydroxybenzoate, ethyl ester, propyl ester, butyl ester containing interior target extraction solution respectively;
The preparation of C, sample solution: use containing interior target extraction solution extraction flavoring essence fragrance sample, obtain sample solution after crossing organic phase filter membrane;
D, Ultra Performance Liquid Chromatography-tandem mass spectrometer analysis: utilize Ultra Performance Liquid Chromatography-tandem mass spectrometer to carry out detection to standard solution and sample solution respectively and analyze;
The calculating of seven kinds of composition salicylic acids, sodium cyclohexylsulfamate, benzoic acid, methyl p-hydroxybenzoate, ethyl ester, propyl ester, butyl ester content in E, flavoring essence spices;
Wherein, the liquid-phase chromatographic analysis condition described in D step is: chromatographic column adopts C18,1.7 μm, 2.1 × 100mm chromatographic column; Mobile phase is methyl alcohol A and 0.05% aqueous formic acid B; Flow velocity: 0.4mL/min; Sample size: 5 μ L; Column temperature: 40 DEG C; Sample temperature: 10 DEG C; Adopt gradient elution program, namely initial A is 10%, B, and A is 35%, B when being 90%, 1min is 65%, during 4min, A is 65%, B, and initial A is 90%, B when being 35%, 6min when being 10%, 7min that A is 90%, when B is 10%, 8min, A is 10%, B, and A is 10%, B when being 90%, 10min is 90%; Described Mass Spectrometry Conditions is for adopting electric spray ion source (ESI) negative ion mode, scan mode is multiple-reaction monitoring pattern, electron spray voltage is-4500V, ion source temperature 600 DEG C, gas curtain gas: 25Psi, atomization gas: 55Psi, auxiliary heating gas: 50Psi, the quota ion of salicylic acid, sodium cyclohexylsulfamate, benzoic acid, methyl p-hydroxybenzoate, ethyl ester, propyl ester, butyl ester and salicylic acid-d4 is to being respectively: m/z92.9,79.9,77.0,92.0,91.9,92.0,92.1,96.9.
2. the method for seven kinds of composition Simultaneously test in flavoring essence spices according to claim 1, it is characterized in that the preparation of standard solution described in step B is: take salicylic acid, sodium cyclohexylsulfamate, benzoic acid, methyl p-hydroxybenzoate, ethyl ester, propyl ester, each 20mg of butyl ester respectively, be transferred in the brown volumetric flask of 100mL after dissolving with methyl alcohol, be settled to scale, obtain single standard storing solution respectively; Take salicylic acid-d410mg, be transferred in the brown volumetric flask of 50mL after dissolving with methyl alcohol, methanol constant volume, to scale, obtains interior mark storing solution; Get respectively in the brown volumetric flask of single standard storing solution 0.5 ~ 2mL to 50mL, by methanol constant volume to scale, obtain one-level mixed standard solution; Get in the brown volumetric flask of interior mark storing solution 1mL to 50mL, by methanol constant volume to scale, obtain mark standard solution in one-level; Accurately pipette the one-level mixed standard solution of 0.1mL, 0.5mL, 1mL, 2mL, 5mL respectively in the brown volumetric flask of 50mL, each brown volumetric flask all adds mark standard solution in 1mL one-level, is settled to scale, obtains series standard solution with extraction solution.
3. the method for seven kinds of composition Simultaneously test in flavoring essence spices according to claim 1, is characterized in that getting mark storing solution in 0.4mL and, in the brown volumetric flask of 1L, is settled to scale with extraction solution, obtain containing interior target extraction solution.
4. the method for seven kinds of composition Simultaneously test in flavoring essence spices according to claim 1 or 3, is characterized in that described is salicylic acid-d4 containing the internal standard compound in interior target extraction solution.
5. the method for seven kinds of composition Simultaneously test in flavoring essence spices according to claim 1, it is characterized in that the preparation method of sample solution described in step C is: take 0.5g sample in 50mL tool plug conical flask, accurately add 25mL containing interior target extraction solution, with 150r/min oscillation extraction 20min, get supernatant and cross organic phase filter membrane, filtrate is sample solution.
6. the method for seven kinds of composition Simultaneously test in flavoring essence spices according to claim 1 or 5, is characterized in that described organic phase filter membrane is 0.22 μm of polyethersulfone membranes.
7. the method for seven kinds of composition Simultaneously test in flavoring essence spices according to claim 1, it is characterized in that the calculating of content described in E step is: first carry out regretional analysis with the chromatographic peak area of the object detected by standard solution and internal standard compound than its respective concentration ratio corresponding and obtain typical curve linear equation, the chromatographic peak area of the object then sample solution detected, substitute into typical curve linear equation, namely obtain the content of salicylic acid in sample, sodium cyclohexylsulfamate, benzoic acid, methyl p-hydroxybenzoate, ethyl ester, propyl ester, butyl ester.
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| CN105699475A (en) * | 2016-01-14 | 2016-06-22 | 中国检验检疫科学研究院 | Method for quick detection of parabens preservative forbidden in cosmetics |
| CN105891374A (en) * | 2016-06-13 | 2016-08-24 | 广西中烟工业有限责任公司 | Detection method for measuring eight preservatives in reconstituted tobaccos simultaneously |
| CN106290642A (en) * | 2016-08-13 | 2017-01-04 | 浙江省海洋水产研究所 | A kind of method of sodium cyclamate in Ultra Performance Liquid Chromatography mass spectrometric determination fishery technology |
| CN106338570A (en) * | 2016-08-13 | 2017-01-18 | 浙江省海洋水产研究所 | Improved method for determination of sodium cyclamate in aquatic processed product |
| CN106950313A (en) * | 2017-04-12 | 2017-07-14 | 中国农业科学院果树研究所 | The method for detecting 3 kinds of sweeteners in fruit simultaneously using Ultra Performance Liquid Chromatography tandem mass spectrometry |
| CN110824064B (en) * | 2019-11-29 | 2022-07-01 | 江苏中烟工业有限责任公司 | Method for determining main sweetener in edible essence and flavor by adopting HPLC-MS/MS |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102944626A (en) * | 2012-11-28 | 2013-02-27 | 国家烟草质量监督检验中心 | Method for detecting content of four disabled components in flavors and fragrances |
-
2014
- 2014-07-28 CN CN201410362880.7A patent/CN104297359B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102944626A (en) * | 2012-11-28 | 2013-02-27 | 国家烟草质量监督检验中心 | Method for detecting content of four disabled components in flavors and fragrances |
Non-Patent Citations (2)
| Title |
|---|
| 超高效液相色谱法同时测定香精香料中14种禁限用物质;李晶 等;《色谱》;20120828;第30卷(第8期);实验部分 * |
| 超高效液相色谱法快速分离测定糖精钠、芝麻酚、酸性橙Ⅱ 和碱性嫩黄O;李晶 等;《光谱实验室》;20130531;第30卷(第3期);结果与讨论部分第3.2节 * |
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