CN108152388A - The detection method of fluorescent whitening agent substance in a kind of lotus nut starch - Google Patents
The detection method of fluorescent whitening agent substance in a kind of lotus nut starch Download PDFInfo
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- CN108152388A CN108152388A CN201711203381.3A CN201711203381A CN108152388A CN 108152388 A CN108152388 A CN 108152388A CN 201711203381 A CN201711203381 A CN 201711203381A CN 108152388 A CN108152388 A CN 108152388A
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- sample
- fluorescent brightening
- substance
- prepare liquid
- brightening substance
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
Abstract
The present invention provides a kind of detection method of fluorescent brightening substance in lotus nut starch, including：Sample preparation；Sample extraction；Sample purification；Prepare liquid is subjected to analysis detection using ultra performance liquid chromatography tandem mass spectrometry, the detection of ultra performance liquid chromatography tandem mass spectrum is obtained, the peak area of ratio and fluorescent brightening substance substitution following formula point is taken to calculate, to obtain the measured value of fluorescent brightening substance in prepare liquid；
Description
Technical field
Present invention relates particularly to a kind of detection methods of fluorescent brightening substance in lotus nut starch.
Background technology
Lotus seeds are the seeds of Nymphaeceae aquatic herbaceous plant lotus, are a kind of time-honored natural health-care products in China, battalion
It is abundant to support value, has to clear away heart-fire and be amusing, stomach controlling nocturnal emission with astringent drugs, nourishing vigour and other effects are mended in mental-tranquilization.Because it is with abundant nutriture value
Value and excellent health-care effect are favored by more and more people.Since fresh lotus seed is not easy to maintain, after lotus seeds harvesting
It is general to dry preservation, but dry lotus seeds are more difficult cooked, it is edible for convenience, it can be ground and be made " lotus nut starch " in lotus seeds production
Product is eaten for consumer.Since dry lotus seeds store improper moisture-sensitive, the lotus seeds to make moist easily turn to be yellow, in addition, old lotus seeds
Color is also partially yellow, and therefore, indivedual bad enterprises is reduce cost, using fluorescent brightening substance in lotus seeds process, to carry
The quality of high lotus nut starch.
Fluorescent brightening substance Fluorescent Brightener 33 (FB33) are a kind of fluorescent dyes, can be absorbed not
The organic compound of visible blue or bluish violet fluorescence is inspired after visible ultraviolet light again, there is potential cause on toxicity
It is carcinous, after being absorbed by the body major injury may be caused to liver, kidney of human body etc..Fluorescent brightening substance FB 33 is mainly used for
Paper-plastic package material to improve the whiteness of product and gorgeous degree, is found illegal retailer and is used in lotus seeds product in recent years.
China is lotus seeds producing and selling and big export country, and as lotus seeds product market becomes increasingly prosperous, the quality security problem of lotus seeds is increasingly
It highlights, for lotus nut starch mainly as middle-aged and old health's food and infant food, safety is especially pronounced.Therefore it studies and makes
The method for quantitatively determining for determining fluorescent brightening substance in lotus nut starch is of great significance.At present, both at home and abroad in relation to fluorescent brightening substance
The report of detection, is concentrated mainly in paper and detergent, and has no the detection method report of fluorescent brightening substance FB33.This
Outside, it is looked into via standards such as ISO, ASTM, GB, SN and newly has no that relevant criterion is reported, related patents report is also had no through patent network inquiry
Road.Therefore it is badly in need of the detection method of fluorescent brightening substance in a kind of easy, quick lotus nut starch of exploitation.
Invention content
The technical problem to be solved in the present invention is to provide a kind of detection method of fluorescent brightening substance in lotus nut starch.
The invention is realized in this way：The detection method of fluorescent brightening substance, includes the following steps in a kind of lotus nut starch：
(1) sample preparation：Sample is fully crushed with pulverizer, mixing, acquisition prepares sample, is preserved under room temperature, spare；
(2) sample extraction：1g is weighed in sample from preparing, 65% methanol-water solutions of 10mL are added in, on liquid blending device
Mixing 1min, 70 DEG C of water bath sonicators extract 30min, and 4000r/min centrifugation 5min obtain sample supernatant；
(3) sample purification：Weak anionic solid-phase extraction column with 3mL methanol and 3mL water is activated respectively, is taken on 1mL samples
Clear liquid crosses column, then is eluted with 3mL water and 3mL methanol, and control Solid Phase Extraction flow velocity discards whole effluxes in 1mL/min；Most
Afterwards with the solid-phase extraction column after 2.0% ammonia water-methanol solution elutions of 10mL, whole effluxes are collected, are blown in 50 DEG C of nitrogen
It is near dry, use 1mL30:70:Acetonitrile, 5mmol/L ammonium acetates and the dissolving of formic acid mixed liquor of 0.1 (volume ratio), cross 0.22 μm of filter membrane,
Obtain prepare liquid；
(4) analysis detection is carried out using ultra performance liquid chromatography-tandem mass spectrometry, it is i.e. glimmering to obtain measured object in prepare liquid
The response of light whitening substance is chosen the corresponding standard working solution of response according to the response condition of measured object in prepare liquid and is carried out
Chromatography, standard working solution are equipped with comprising five concentration gradients including zero, and fluorescence in standard working solution and prepare liquid
The response of whitening substance should all be in instrument linear response range, and sets blank control simultaneously；
The condition of the ultra performance liquid chromatography-tandem mass spectrum is：
A. ultra performance liquid chromatography:
Chromatographic column：Thermo Syncronnic C18 columns, 50mm × 2.1mm, 1.7 μm；Flow velocity：0.3mL/min；Sample introduction
Amount：10μL；Column temperature：30℃；Gradient elution program is as follows：
| Time/Min | 5mmol/L ammonium acetate buffer solutions/% | Acetonitrile/% | Methanol/% |
| 0 | 80 | 10 | 10 |
| 1.00 | 80 | 10 | 10 |
| 2.00 | 30 | 60 | 10 |
| 5.00 | 30 | 60 | 10 |
| 5.01 | 80 | 10 | 10 |
| 6.00 | 80 | 10 | 10 |
B. Mass Spectrometry Conditions：
Ion source：Electron spray ESI, cation；Scan mode：Multiple-reaction monitoring MRM；Atomization gas, curtain gas, auxiliary heating
Gas, collision gas are high pure nitrogen；Monitoring ion pair, quota ion pair go to cluster voltage, collision gas energy, collision cell outlet
Voltage is as follows：
(5) the peak face for point taking ratio and fluorescent brightening substance for being obtained the detection of ultra performance liquid chromatography-tandem mass spectrum
Product substitutes into following formula (1) and is calculated, to obtain the measured value of fluorescent brightening substance in prepare liquid；
Wherein：
Fluorescent brightening substance fluorescent brightening substance FB33 residual contents, mg/kg in X-sample；
The peak area of fluorescent brightening substance FB33 in A-prepare liquid；
The peak area of fluorescent brightening substance FB33 in As-standard working solution；
Fluorescent brightening substance FB33 concentration, mg/L in c-standard working solution；
The final constant volume of V-prepare liquid, mL；
The quality of m-sample, g；
R-point take ratio.
The advantage of the invention is that：Blank of the China in lotus nut starch in the detection technique of fluorescent brightening substance has been filled up,
And have the advantages that easily operated and detection accuracy is high.
Specific embodiment
The detection method of fluorescent brightening substance, includes the following steps in a kind of lotus nut starch：
(1) sample preparation：Representative sample is taken, is fully crushed with pulverizer, mixing, experiment is divided into two parts, is packed into clean
Container seals and carries out mark, is preserved under room temperature, spare；
(2) sample extraction：About 1g (being accurate to 0.01g) is weighed in sample in 15mL tool plug centrifuge tubes from preparing, is added in
65% methanol-water solutions of 10mL, in mixing 1min on liquid blending device, 70 DEG C of water bath sonicators extract 30min, 4000r/min from
Heart 5min, obtains extracting solution；
(3) sample purification：Weak anionic solid-phase extraction column 3mL methanol and 3mL water are activated, take 1mL sample supernatants
Column is crossed, then is eluted with 3mL water and 3mL methanol, control Solid Phase Extraction flow velocity discards whole effluxes in 1mL/min.Finally use
2.0% ammonia water-methanol solution elution columns of 10mL are collected whole effluxes in 10mL scale colorimetric cylinders, are blown in 50 DEG C of nitrogen
It is done near, uses 1mL30:70:Acetonitrile, 5mmol/L ammonium acetates and the dissolving of formic acid mixed liquor of 0.1 (volume ratio), cross film, are treated
Survey liquid；
(4) analysis detection is carried out using ultra performance liquid chromatography-tandem mass spectrometry, it is i.e. glimmering to obtain measured object in prepare liquid
The response of light whitening substance is chosen the corresponding standard working solution of response according to the response condition of measured object in prepare liquid and is carried out
Chromatography, standard working solution are equipped with comprising five concentration gradients including zero, and fluorescence in standard working solution and prepare liquid
The response of whitening substance should all be in instrument linear response range, and sets blank control simultaneously；
The condition of the ultra performance liquid chromatography-tandem mass spectrum is：
A. liquid chromatogram:
Chromatographic column：Thermo Syncronnic C18 columns, 50mm × 2.1mm, 1.7 μm；Flow velocity：0.3mL/min；Sample introduction
Amount：10μL；Column temperature：30℃；Gradient elution program is as follows：
| Time/Min | 5mmol/L ammonium acetate buffer solutions/% | Acetonitrile | Methanol |
| 0 | 80 | 10 | 10 |
| 1.00 | 80 | 10 | 10 |
| 2.00 | 30 | 60 | 10 |
| 5.00 | 30 | 60 | 10 |
| 5.01 | 80 | 10 | 10 |
| 6.00 | 80 | 10 | 10 |
B. Mass Spectrometry Conditions：
Ion source：Electron spray ESI, cation；Scan mode：Multiple-reaction monitoring MRM；Atomization gas, curtain gas, auxiliary heating
Gas, collision gas are high pure nitrogen；Monitoring ion pair, quota ion pair go to cluster voltage, collision gas energy, collision cell outlet
Voltage is as follows：
(5) ultra performance liquid chromatography-tandem mass spectrum detection is obtained into point peak area for taking ratio and fluorescent brightening substance
It substitutes into following formula (1) to be calculated, to obtain the measured value of fluorescent brightening substance in prepare liquid；
Wherein：
Fluorescent brightening substance fluorescent brightening substance FB33 residual contents, mg/kg in X-sample；
The peak area of fluorescent brightening substance FB33 in A-prepare liquid；
The peak area of fluorescent brightening substance FB33 in As-standard working solution；
Fluorescent brightening substance FB33 concentration, mg/L in c-standard working solution；
The final constant volume of V-prepare liquid, mL；
The quality of m-sample, g；
R-point take ratio.
Embodiment 1：Sample to be tested --- lotus nut starch
1.1 sample preparation：Representative sample is taken, is fully crushed with pulverizer, mixing, clean container is packed into and seals and carry out
Mark, as sample.Sample preparation procedure must be prevented from the variation that sample was contaminated or occurred residuals content, be protected under room temperature
It deposits.
1.2 backgrounds are tested：It is respectively weighed into six 50mL tool plug centrifuge tubes described in 1.00g (being accurate to 0.01g) 1.1
Sample is then operated successively according to step in the specific embodiment of the invention (2), step (3) and step (4), is finally counted
Each actual measured value and the average value for calculating gained are as shown in table 1, which is background values.
The background values determination data of fluorescent brightening substance FB33 in 1 lotus nut starch of table
1.3 verifications one：Add 0.1mg/kg fluorescent brightening substances FB33
The sample in 1.00g (being accurate to 0.01g) 1.1 is respectively weighed into six 15mL tool plug centrifuge tubes (to be specifically shown in
Sample weighting amount in table 2), the fluorescent brightening substance FB33 standard solution 0.1mL of 1mg/L are then added into each centrifuge tube, are connect
It and is operated successively according to step in the present invention (2), step (3) and step (4), finally calculate each actual measured value of gained
It is listed in Table 2 below.
The related data of the fluorescent brightening substance FB33 of 0.1mg/kg is added in 2 lotus nut starch sample of table
1.4 verifications two：Add 0.5mg/kg fluorescent brightening substances FB33
The sample in 1.00g (being accurate to 0.01g) 1.1 is respectively weighed into six 50mL tool plug centrifuge tubes (to be specifically shown in
Sample weighting amount in table 3), the fluorescent brightening substance FB33 standard solution 0.25mL of 2mg/L are then added into each centrifuge tube, are connect
It and is operated successively according to step in the present invention (2), step (3) and step (4), and the last each reality for calculating gained is surveyed
Definite value is listed in Table 3 below.
The rate of recovery data of the fluorescent brightening substance FB33 of 0.5mg/kg are added in 3 lotus nut starch sample of table
By above-mentioned experimental result it is found that the present invention is applied to fluorescent brightening substance FB33 contents in detection lotus nut starch sample
When, lower limit of measurement is：0.1mg/kg, rate of recovery 80-110%, standard curve linear relationship is good in the range of 0.1~2mg/L
Good, correlation coefficient r is more than 0.999.
The detection method that can determine whether out the present invention from the rate of recovery in respective verification result and the size of RSD not only may be used
Row, and accuracy is high.
Although specific embodiments of the present invention have been described above, those familiar with the art should manage
Solution, our described specific embodiments are merely exemplary rather than for the restriction to the scope of the present invention, are familiar with this
The equivalent modification and variation that the technical staff in field is made in the spirit according to the present invention, should all cover the present invention's
In scope of the claimed protection.
Claims (1)
1. a kind of detection method of fluorescent brightening substance in lotus nut starch, it is characterised in that：Include the following steps：
(1) sample preparation：Sample is fully crushed with pulverizer, mixing, acquisition prepares sample, is preserved under room temperature, spare；
(2) sample extraction：1g is weighed in sample from preparing, 65% methanol-water solutions of 10mL are added in, in mixing on liquid blending device
1min, 70 DEG C of water bath sonicators extract 30min, and 4000r/min centrifugation 5min obtain sample supernatant；
(3) sample purification：Weak anionic solid-phase extraction column with 3mL methanol and 3mL water is activated respectively, takes 1mL sample supernatants
Column is crossed, then is eluted with 3mL water and 3mL methanol, control Solid Phase Extraction flow velocity discards whole effluxes in 1mL/min；Finally use
Solid-phase extraction column after 2.0% ammonia water-methanol solution elutions of 10mL is collected whole effluxes, is blown to closely in 50 DEG C of nitrogen
It is dry, it is 30 with 1mL volume ratios:70:0.1 acetonitrile, 5mmol/L ammonium acetates and the dissolving of formic acid mixed liquor, crosses 0.22 μm of filter membrane, obtains
Obtain prepare liquid；
(4) analysis detection is carried out using ultra performance liquid chromatography-tandem mass spectrometry, is increased with obtaining measured object i.e. fluorescence in prepare liquid
The response of white substance chooses the corresponding standard working solution of response according to the response condition of measured object in prepare liquid and carries out chromatography
Analysis, standard working solution are equipped with comprising five concentration gradients including zero, and fluorescent brightening in standard working solution and prepare liquid
The response of substance should all be in instrument linear response range, and sets blank control simultaneously；
The condition of the ultra performance liquid chromatography-tandem mass spectrum is：
A. ultra performance liquid chromatography:
Chromatographic column：Thermo Syncronnic C18 columns, 50mm × 2.1mm, 1.7 μm；Flow velocity：0.3mL/min；Sample size：10
μL；Column temperature：30℃；Gradient elution program is as follows：
B. Mass Spectrometry Conditions：
Ion source：Electron spray ESI, cation；Scan mode：Multiple-reaction monitoring MRM；Atomization gas, curtain gas, auxiliary heating gas,
Collision gas is high pure nitrogen；Monitoring ion pair, quota ion pair remove cluster voltage, collision gas energy, collision cell exit potential
It is as follows：
(5) the peak area generation for point taking ratio and fluorescent brightening substance for being obtained the detection of ultra performance liquid chromatography-tandem mass spectrum
Enter following formula (1) to be calculated, to obtain the measured value of fluorescent brightening substance in prepare liquid；
Wherein：
Fluorescent brightening substance fluorescent brightening substance FB33 residual contents, mg/kg in X-sample；
The peak area of fluorescent brightening substance FB33 in A-prepare liquid；
The peak area of fluorescent brightening substance FB33 in As-standard working solution；
Fluorescent brightening substance FB33 concentration, mg/L in c-standard working solution；
The final constant volume of V-prepare liquid, mL；
The quality of m-sample, g；
R-point take ratio.
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| CN201711203381.3A CN108152388A (en) | 2017-11-27 | 2017-11-27 | The detection method of fluorescent whitening agent substance in a kind of lotus nut starch |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711203381.3A CN108152388A (en) | 2017-11-27 | 2017-11-27 | The detection method of fluorescent whitening agent substance in a kind of lotus nut starch |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102175784B (en) * | 2011-01-19 | 2012-09-26 | 浙江出入境检验检疫局检验检疫技术中心 | Method for synchronously detecting 54 medicament residues in pork by virtue of solid phase extraction-liquid chromatogram-mass spectrum/mass spectrometry |
| CN103201265A (en) * | 2010-11-12 | 2013-07-10 | 先正达参股股份有限公司 | Novel microbiocides |
| CN104931606A (en) * | 2015-05-26 | 2015-09-23 | 三明出入境检验检疫局综合技术服务中心 | Detection method of fluorescence whitening agent in food packaging plastic material |
| CN105628806A (en) * | 2015-12-22 | 2016-06-01 | 三明出入境检验检疫局综合技术服务中心 | Detection method for cyantraniliprole in honey |
-
2017
- 2017-11-27 CN CN201711203381.3A patent/CN108152388A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103201265A (en) * | 2010-11-12 | 2013-07-10 | 先正达参股股份有限公司 | Novel microbiocides |
| CN102175784B (en) * | 2011-01-19 | 2012-09-26 | 浙江出入境检验检疫局检验检疫技术中心 | Method for synchronously detecting 54 medicament residues in pork by virtue of solid phase extraction-liquid chromatogram-mass spectrum/mass spectrometry |
| CN104931606A (en) * | 2015-05-26 | 2015-09-23 | 三明出入境检验检疫局综合技术服务中心 | Detection method of fluorescence whitening agent in food packaging plastic material |
| CN104931606B (en) * | 2015-05-26 | 2017-06-06 | 三明出入境检验检疫局综合技术服务中心 | The detection method of fluorescent whitening agent in package plastics of food material |
| CN105628806A (en) * | 2015-12-22 | 2016-06-01 | 三明出入境检验检疫局综合技术服务中心 | Detection method for cyantraniliprole in honey |
Non-Patent Citations (3)
| Title |
|---|
| CHENGJIANG ZHANG 等: "Acylhydrazone bond dynamic covalent polymer gel monolithic column online coupling to high-performance liquid chromatography for analysis of sulfonamides and fluorescent whitening agents in food", 《JOURNAL OF CHROMATOGRAPHY A》 * |
| 张建莹 等: "超高效液相色谱-串联质谱法检测食用菌中荧光增白剂", 《食品安全质量检测学报》 * |
| 葛广周 等: "《染料索引》中部分荧光增白剂的化学结构（II）", 《染料与染色》 * |
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