CN102221582B - Method for rapidly detecting rhodamine B in chafing dish materials - Google Patents
Method for rapidly detecting rhodamine B in chafing dish materials Download PDFInfo
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- CN102221582B CN102221582B CN 201110082949 CN201110082949A CN102221582B CN 102221582 B CN102221582 B CN 102221582B CN 201110082949 CN201110082949 CN 201110082949 CN 201110082949 A CN201110082949 A CN 201110082949A CN 102221582 B CN102221582 B CN 102221582B
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Abstract
The invention discloses a method for rapidly detecting rhodamine B in chafing dish materials. The method comprises the following steps: weighting a certain amount of chafing dish materials required to be detected, a saturated sodium chloride solution, acetonitrile and hexane for mixing to place in a centrifuge tube with a plug, oscillating and extracting for 10 to 20 minutes, centrifuging at a speed of 4000 to 6000 r/min for 4 to 10 minutes, absorbing 1 to 2 mL of acetonitrile layer by an injector, passing through an organic millipore filtration with a diameter of 0.2 mum to obtain a purified chafing dish materials; a liquid chromatography is employed for an ion exchange chromatography-fluorescence detection to the purified chafing dish materials, a liquid chromatography of the chafing dish materials can be obtained, whether rhodamine B exists or not and the quantification are determined according to the liquid chromatography. The method for rapidly detecting rhodamine B in chafing dish materials provided in the invention has the advantages of rapidity, sensitivity, accuracy, low cost, strong specificity and strong practicality, which is suitable for the rapid detection of rhodamine B in chafing dish materials and raw materials.
Description
Technical field
The invention belongs to the food inspection technical field, relate to a kind of detection method of food component, be specifically related to the method for quick of rhodamine B in a kind of chafing dish bottom flavorings.
Background technology
Rhodamine B claims again rhodamine B, rose-red, pollen is red etc., English name is Rhodamine B, it is a kind of artificial synthetic industrial dye, be mainly used in textile, leather and fur products, woodwork, the dyeing of coloured glass etc., the same with tonyred have carcinogenesis to human body, listed in the non-edible material from soybeans blacklist of the illegal interpolation of possibility in first food in 2008 by ministry of Health of China, but because rhodamine B has cheap, color and luster is red gorgeous, the characteristics such as stability is strong, often by the colorant of illegal retailer as the substitute food product adjuvant, serious harm people's safe diet.
Chafing dish is China's popular cuisines among the people, be popular in all parts of the country, formed at present huge diet industry, chafing dish bottom flavorings is one of indispensable raw material in the chafing dish diet, the chafing dish bottom flavorings of main flow is mainly by capsicum, bean cotyledon, butter, the plant wet goods consists of, some lawless persons are in order to pursue the color and luster of product, in capsicum, illegally in the raw material such as bean cotyledon or the chafing dish bottom flavorings product add the industrial dye rhodamine B, harm people's safe diet, Spring Festival in 2011, Shenzhen, Chongqing, Hebei, the rhodamine B of illegal interpolation is found on the ground such as Sichuan from chafing dish bottom flavorings, aggravated the worry of people to rhodamine B, rhodamine B in the chafing dish bottom flavorings has been carried out fast detecting have positive meaning.
The detection method of rhodamine B mainly contains High Performance Liquid Chromatography with Fluorescence Detection, high performance liquid chromatography-uv detection method, Liquid Chromatography-Tandem Mass Spectrometry in the food at present, but the sample pre-treatments of these methods all needs to adopt Solid-Phase Extraction or gel permeation chromatography to purify, process is complicated, cost is high, the cycle is long, testing process adopts reverse C18 chromatographic column to separate, specificity is poor, easily produce and disturb, and do not have special detection method for the chafing dish bottom flavorings sample.
Summary of the invention
The method for quick that the purpose of this invention is to provide rhodamine B in a kind of chafing dish bottom flavorings, the sample pre-treatments that has solved the detection method existence of rhodamine B in the existing chafing dish bottom flavorings all needs to adopt Solid-Phase Extraction or gel permeation chromatography to purify, process is complicated, cost is high, the cycle is long, and testing process adopts reverse C18 chromatographic column to separate, specificity is poor, easily produces the problem of disturbing.
The technical solution adopted in the present invention is, the method for quick of rhodamine B in a kind of chafing dish bottom flavorings is specifically implemented according to following steps:
Step 1: take by weighing a certain amount of chafing dish bottom flavorings to be detected, quality-volumetric concentration according to the chafing dish bottom flavorings to be detected that takes by weighing and saturated nacl aqueous solution is that 250-400g/L takes by weighing saturated nacl aqueous solution, quality-volumetric concentration according to the chafing dish bottom flavorings to be detected that takes by weighing and acetonitrile is that 100-200g/L takes by weighing acetonitrile, quality-volumetric concentration according to the chafing dish bottom flavorings to be detected that takes by weighing and normal hexane is that 100-200g/L takes by weighing normal hexane, with the chafing dish bottom flavorings to be detected that takes by weighing, saturated nacl aqueous solution, acetonitrile and normal hexane mixing place tool plug centrifuge tube, vibration 10～20min, with the centrifugal 4～10min of the speed of 4000～6000r/min, draw 1～2mL acetonitrile layer with syringe, the acetonitrile layer of drawing is crossed the organic miillpore filter of 0.2 μ m, the chafing dish bottom flavorings after being purified;
Step 2: adopt the chafing dish bottom flavorings after the purification that liquid chromatograph obtains step 1 to carry out ion-exchange chromatography-fluoroscopic examination, obtain the liquid chromatogram of chafing dish bottom flavorings, judge according to liquid chromatogram whether rhodamine B and quantitative is arranged in the chafing dish bottom flavorings.
Characteristics of the present invention also are,
Wherein ion-exchange chromatography-the fluoroscopic examination in the step 2 arranges detected parameters: SCX strong cation exchange chromatography post: column length 250mm, column internal diameter 4.6mm, packing material size 5 μ m; Mobile phase: volume ratio is 4: 6 acetonitrile-0.1% ammonia spirit, isocratic elution; Flow velocity: 0.8～1.2mL/min; Column temperature: 30～40 ℃; Sample size: 10～100 μ L; Excitation wavelength: 548～552nm, emission wavelength: 578～582nm.
Wherein judge that according to liquid chromatogram the criterion whether rhodamine B is arranged in the chafing dish bottom flavorings is in the step 2: have chromatographic peak to occur if the liquid chromatogram of sample goes out the peak position in rhodamine B standard solution chromatogram, and signal to noise ratio (S/N ratio) is greater than 5, then contain rhodamine B in the judgement sample, do not have chromatographic peak to occur if the liquid chromatogram of sample goes out the peak position in rhodamine B standard solution chromatogram, then do not detect rhodamine B in the sample.
Wherein quantitative employing calibration curve method or the one point external standard method of rhodamine B in the step 2.
The invention has the beneficial effects as follows, sample extraction, purification were finished in a step, removed Solid-Phase Extraction or the gel infiltration purification process in the classic method from, save time for sample pretreatment more than 5 times, reduce the pre-treatment cost more than 10 times, utilize the strong ion-exchange chromatography sample separation of selectivity, and in conjunction with the strong fluorescence detector detection of specificity, can significantly improve antijamming capability, avoid false positive results, improve the accuracy of testing result.Sample of the complete detection of this detection method only needs less than the 40min time, about 2 yuan of reagent costs, detection limit can reach 5 μ g/kg, sense cycle is short, testing cost is low, testing result is accurate, highly sensitive, be fit to manufacturing enterprise and administrative authority and carry out the product quality detection, when batch samples detects, more can embody detection speed and the testing cost advantage of this method.
Description of drawings
Fig. 1 is the chemical structural formula of rhodamine B;
Fig. 2 is the liquid chromatogram of the rhodamine B standard solution of 2ng/mL;
Fig. 3 is the reagent blank liquid chromatogram;
Fig. 4 is chafing dish bottom flavorings sample liquid chromatogram;
Fig. 5 is that chafing dish bottom flavorings sample mark-on level is the liquid chromatogram of 10 μ g/kg;
Fig. 6 is the visible absorption collection of illustrative plates of rhodamine B.
Embodiment
The present invention is described in detail below in conjunction with the drawings and specific embodiments.
The method for quick of rhodamine B in the chafing dish bottom flavorings of the present invention, specifically implement according to following steps:
Step 1: take by weighing a certain amount of chafing dish bottom flavorings to be detected, extract and purify, quality-volumetric concentration according to the chafing dish bottom flavorings to be detected that takes by weighing and saturated nacl aqueous solution is that 250-400g/L takes by weighing saturated nacl aqueous solution, quality-volumetric concentration according to the chafing dish bottom flavorings to be detected that takes by weighing and acetonitrile is that 100-200g/L takes by weighing acetonitrile, quality-volumetric concentration according to the chafing dish bottom flavorings to be detected that takes by weighing and normal hexane is that 100-200g/L takes by weighing normal hexane, mix and place tool plug centrifuge tube, mechanical shaking extraction 10～20min, centrifugal 4～the 10min of 4000～6000r/min, draw 1～2mL acetonitrile layer (middle layer) with syringe, cross the organic miillpore filter of 0.2 μ m, the chafing dish bottom flavorings sample after being purified;
Step 2: the employing liquid chromatograph carries out ion-exchange chromatography-fluoroscopic examination, detected parameters is set is: chromatographic column: SCX strong cation exchange chromatography post (column length 250mm, column internal diameter 4.6mm, packing material size 5 μ m), or suitable person; Mobile phase: acetonitrile-0.1% ammonia spirit (4+6, volume ratio) isocratic elution; Flow velocity: 0.8～1.2mL/min; Column temperature: 30～40 ℃; Sample size: 10～100 μ L; Excitation wavelength (Ex) 548～552nm, emission wavelength (Em) 578～582nm, the chafing dish bottom flavorings sample that the upper step was obtained detects, obtain the liquid chromatogram of chafing dish bottom flavorings sample, if going out the peak position in rhodamine B standard solution chromatogram, the liquid chromatogram of sample have chromatographic peak to occur, and signal to noise ratio (S/N ratio) is greater than 5, but then contain rhodamine B in the judgement sample, otherwise, do not have chromatographic peak to occur if the liquid chromatogram of sample goes out the peak position in rhodamine B standard solution chromatogram, then do not detect rhodamine B in the sample.Rhodamine B in the sample adopts external standard method to carry out quantitatively, and quantivative approach can be selected calibration curve method or one point external standard method.
Embodiment 1
Take by weighing 1g (being accurate to 0.01g) and do not contain the chafing dish bottom flavorings sample of rhodamine B in 50mL tool plug centrifuge tube, add 50ng rhodamine B standard, add 4.0mL saturated nacl aqueous solution, 10mL acetonitrile, 10mL normal hexane, mechanical shaking extraction 10min, the centrifugal 10min of 4000r/min, draw about 2mL acetonitrile layer with syringe, cross the organic miillpore filter of 0.2 μ m.Adopt Supelco SCX chromatographic column (column length 250mm during analysis, column internal diameter 4.6mm, packing material size 5 μ m), mobile phase is acetonitrile-0.1% ammonia spirit (4+6, volume ratio), flow velocity 1.0mL/min, 35 ℃ of column temperatures, sample size 50 μ L, excitation wavelength 550nm, emission wavelength 580nm, rhodamine B goes out the peak at 7.1min in the mark-on sample, identical with the appearance time of rhodamine B in the standard solution, the content that utilizes calibration curve method to calculate Luo Dan B in the sample solution is 9.53ng/mL, and the recovery is 95.3%.
Take by weighing 2g (being accurate to 0.01g) and do not contain the chafing dish bottom flavorings sample of rhodamine B in 50mL tool plug centrifuge tube, add 100ng rhodamine B standard, add 5mL saturated nacl aqueous solution, 10mL acetonitrile, 10mL normal hexane, mechanical shaking extraction 15min, the centrifugal 6min of 5000r/min, draw about 1.5mL acetonitrile layer with syringe, cross the organic miillpore filter of 0.2 μ m.Adopt Supelco SCX chromatographic column (column length 250mm during analysis, column internal diameter 4.6mm, packing material size 5 μ m), mobile phase is acetonitrile-0.1% ammonia spirit (4+6, volume ratio), flow velocity 0.8mL/min, 40 ℃ of column temperatures, sample size 100 μ L, excitation wavelength 548nm, emission wavelength 578nm, rhodamine B goes out the peak at 7.5min in the mark-on sample, identical with the appearance time of rhodamine B in the standard solution, the content that utilizes calibration curve method to calculate Luo Dan B in the sample solution is 9.85ng/mL, and the recovery is 98.5%.
Embodiment 3
Take by weighing 3g (being accurate to 0.01g) and do not contain the chafing dish bottom flavorings sample of rhodamine B in 50mL tool plug centrifuge tube, add 150ng rhodamine B standard, add 9mL saturated nacl aqueous solution, 18mL acetonitrile, 18mL normal hexane, mechanical shaking extraction 20min, the centrifugal 4min of 6000r/min, draw about 2mL acetonitrile layer with syringe, cross the organic miillpore filter of 0.2 μ m.Adopt Supelco SCX chromatographic column (column length 250mm during analysis, column internal diameter 4.6mm, packing material size 5 μ m), mobile phase is acetonitrile-0.1% ammonia spirit (4+6, volume ratio), flow velocity 1.2mL/min, 30 ℃ of column temperatures, sample size 10 μ L, excitation wavelength 552nm, emission wavelength 582nm, rhodamine B goes out the peak at 6.1min in the mark-on sample, identical with the appearance time of rhodamine B in the standard solution, the content that utilizes calibration curve method to calculate Luo Dan B in the sample solution is 9.72ng/mL, and the recovery is 97.2%.
Below the present invention will be described from the principle aspect:
The selection of liquid phase chromatogram condition: the chemical structural formula of rhodamine B contains two nitrogen-containing groups that can form positive ion as shown in Figure 1 in its structure, is fit to carry out compartment analysis with cation-exchange chromatography.Reverse C18 chromatographic column is all adopted in traditional rhodamine B analysis, and the C18 chromatographic column mainly relies on the polarity size of compound to separate different compounds, selectivity is low, to get rid of during sample analysis to disturb just must have and purify good sample pretreatment process, can prolong the time of sample detection, rising testing cost.The cation-exchange chromatography post only has chromatogram to keep to compound that can cationization, so specificity is strong, antijamming capability is strong, can simplify determination, so select the cation-exchange chromatography post to analyze rhodamine B.
The mobile phase that cation-exchange chromatography is commonly used is phosphate buffer and organic phase, and the ratio of the pH value by regulating phosphate buffer and organic phase is adjusted appearance time and the peak shape of compound, 0.1mol/L phosphate sodium dihydrogen buffer solution and acetonitrile have been investigated first in the experiment as the situation of mobile phase, the volume ratio of damping fluid and acetonitrile be 1: 1 (because of salinity in the damping fluid higher, the acetonitrile ratio had better not surpass 50%, salt out otherwise can cause, damage chromatographic system), when phosphate sodium dihydrogen buffer solution pH is 3.0, rhodamine B is adsorbed on the cation-exchange chromatography post, can not be eluted, when phosphate sodium dihydrogen buffer solution pH is 5.6, rhodamine B goes out the peak about 13min, but peak shape is fat, sensitivity is low, when adjusting phosphate sodium dihydrogen buffer solution pH is 8.0, the rhodamine B appearance time in advance, peak shape is improved, but the buffer salt system of considering phosphate sodium dihydrogen buffer solution preparation more complicated and high concentration is not suitable for organic solvent (being acetonitrile in this method) direct injected of large volume, also harmful to liquid chromatographic system, selected afterwards 0.1% ammonia spirit and acetonitrile system to test, when 0.1% ammonia spirit and acetonitrile are 1: 1, rhodamine B goes out the peak about 5min, peak shape is sharp-pointed, but appearance time is too early, one little Interference Peaks can appear in a few sample, and 0.1% ammonia spirit and acetonitrile are 3: 2 o'clock, rhodamine B goes out the peak about 7min, peak shape is good, and noiseless, so finally selecting 0.1% ammonia spirit-acetonitrile (3+2) is mobile phase, standard solution, the liquid chromatogram of reagent blank such as Fig. 2, shown in Figure 3.
Then sampling volume is investigated, dissolved standard with acetonitrile, when difference sample introduction 10,20,50,100 μ L, the chromatographic retention of rhodamine B and chromatographic peak profile are the sensitivity that improves detection method without marked difference, select sample introduction 100 μ L.
Used detecting device mainly contained visible light detector and fluorescence detector when rhodamine B detected, the maximum visible absorbance of rhodamine B is 550nm (Fig. 6), fluorescence exciting wavelength is 550nm, the fluorescent emission wavelength is 580nm, when detecting, visible light detector selects the maximum absorption wavelength 550nm of rhodamine B, but the sensitivity of rhodamine B only has 1/2nd of fluoroscopic examination, and the antijamming capability of visible detection is poorer than fluoroscopic examination, so select fluoroscopic examination.
Rhodamine B standard solution (2ng/mL) is pressed the liquid phase chromatogram condition sample introduction that above-mentioned experiment is determined, detection limit by 5 times of signal-noise ratio computation methods, by the quantitative lower bound of 10 times of signal-noise ratio computation methods, the detection limit of method and quantitative lower bound are respectively 0.5ng/mL, 1.0ng/mL.
The selection of extraction and cleaning condition: rhodamine B is soluble in methyl alcohol, acetonitrile, acetone, be slightly soluble in saturated nacl aqueous solution, solubleness is also far below methyl alcohol and acetonitrile in normal hexane, traditional method adopts the rhodamine B in acetone or the methyl alcohol equal solvent extraction food, then adopt aluminium oxide solid-phase extraction column or gel permeation chromatography to purify, operating process is complicated, length consuming time, and cost is high.This detection method is according to the sample characteristics of dissolution properties and the chafing dish bottom flavorings of rhodamine B, methyl alcohol, acetonitrile, three kinds of extractions of acetone solvent have been investigated, owing to contain more grease and some water-soluble substanceses in the chafing dish bottom flavorings, need to consider to remove these materials in the extraction and cleaning process.Because simplicity and the low cost of liquid-liquid extraction, consider that water and normal hexane liquid-liquid extraction purify, and methyl alcohol and acetone and water dissolve each other, also can dissolve each other with normal hexane, need conversion solvent during extracting and purifying, complicated operation is time-consuming, and acetonitrile under the condition that high salt concentration exists can with water stratification, with normal hexane also effectively layering, so select to carry out sample extraction with acetonitrile, when extracting, acetonitrile adds saturated nacl aqueous solution and normal hexane, and carry out liquid liquid in the time of mechanical shaking extraction and distribute purification, centrifugal rear rhodamine B is present in the acetonitrile layer, has greatly saved time for sample pretreatment and cost.
Extraction and cleaning acetonitrile volume and normal hexane volume have been investigated in the experiment, quality-volumetric concentration according to chafing dish bottom flavorings to be detected and saturated nacl aqueous solution is 250-400g/L, with the quality-volumetric concentration of acetonitrile be 100-200g/L, with the quality-volumetric concentration of normal hexane be 100-200g/L, recovery of standard addition to clean-up effect (degreasing) and rhodamine B does not make significant difference, so consider from the angle of saving reagent, select aforementioned proportion to extract and purify.
Investigated in the experiment the concentrated rear constant volume sample detection of acetonitrile layer and acetonitrile layer have been filtered rear direct injected detection dual mode, be concentrated into the acetonitrile extract dried, with 1mL acetonitrile dissolving constant volume, sample detection after filtering, remolding sensitivity acetonitrile layer direct injected can improve 10 times, but increased operating process, raised the pre-treatment cost, prolonged detection time, and the quantitative lower bound of method has reached 5 μ g/kg (when claiming sample 2.0g) during acetonitrile extract direct injected, can satisfy testing requirement fully, need not operating process is complicated, so select acetonitrile layer is filtered rear direct injected.The liquid chromatogram of chafing dish bottom flavorings sample and sample mark-on (the mark-on level is 10 μ g/kg) as shown in Figure 4 and Figure 5.
Linear relationship: the rhodamine B standard intermediate liquid of getting 1.0 μ g/mL, use the acetonitrile stepwise dilution, be mixed with 1.0,2.0,5.0,10.0,20.0,50.0, the rhodamine B series standard working fluid of 100.0ng/mL, by the definite chromatographic condition sample introduction of above-mentioned experiment, and carry out linear fit with chromatographic peak area Y and the mass concentration X of rhodamine B, equation of linear regression is Y=4.56X-0.83, linearly dependent coefficient r is 0.9999, shows that the linear relationship of rhodamine B in 1.0ng/mL～100.0ng/mL concentration range is good.
Recovery of standard addition and Precision Experiment in the chafing dish bottom flavorings: after determining detection method, take the chafing dish bottom flavorings that do not contain rhodamine B as tested object, carry out recovery of standard addition experiment and Precision Experiment, with the applicability of investigation method.Adopt 5 μ g/kg, 10 μ g/kg, three mark-on levels of 20 μ g/kg, claim sample 2.0g, add respectively 10ng, 20ng, 40ng rhodamine B standard, each mark-on level repeats 6 times, recovery of standard addition and Precision Experiment result are as shown in table 1, and the recovery of standard addition of rhodamine B is in 76.7%～105.5% scope, and recovery relative standard deviation is lower than 8.6%, the recovery and reappearance are good, can satisfy testing requirement fully.
Rhodamine B recovery of standard addition experimental result (n=6) in the negative chafing dish bottom flavorings of table 1
Recovery of standard addition experiment in capsicum and the thick broad-bean sauce: by the detection method of determining, take the capsicum that do not contain rhodamine B and thick broad-bean sauce as tested object, carry out the recovery of standard addition experiment, with the applicability of investigation method to these two kinds of samples.Minimum mark-on level 5 μ g/kg carry out mark-on by the chafing dish bottom flavorings sample, claim sample 2.0g, add 10ng rhodamine B standard, capsicum and thick broad-bean sauce sample counterpoise are added with mark 3 times, the recovery of standard addition of capsicum sample is respectively 85.6%, 97.2%, 90.5%, the recovery of standard addition of thick broad-bean sauce sample is 92.8%, 102.4%, 95.3%, and the recovery is all good, can satisfy testing requirement.
Claims (1)
1. the method for quick of rhodamine B in the chafing dish bottom flavorings is characterized in that, specifically implements according to following steps:
Step 1: take by weighing a certain amount of chafing dish bottom flavorings to be detected, quality-volumetric concentration according to the chafing dish bottom flavorings to be detected that takes by weighing and saturated nacl aqueous solution is that 250-400g/L takes by weighing saturated nacl aqueous solution, quality-volumetric concentration according to the chafing dish bottom flavorings to be detected that takes by weighing and acetonitrile is that 100-200g/L takes by weighing acetonitrile, quality-volumetric concentration according to the chafing dish bottom flavorings to be detected that takes by weighing and normal hexane is that 100-200g/L takes by weighing normal hexane, with the chafing dish bottom flavorings to be detected that takes by weighing, saturated nacl aqueous solution, acetonitrile and normal hexane mixing place tool plug centrifuge tube, vibration 10～20min, with the centrifugal 4～10min of the speed of 4000～6000r/min, draw 1～2mL acetonitrile layer with syringe, the acetonitrile layer of drawing is crossed the organic miillpore filter of 0.2 μ m, the chafing dish bottom flavorings after being purified;
Step 2: adopt the chafing dish bottom flavorings after the purification that liquid chromatograph obtains step 1 to carry out ion-exchange chromatography-fluoroscopic examination, obtain the liquid chromatogram of chafing dish bottom flavorings, judge according to liquid chromatogram whether rhodamine B and quantitative is arranged in the chafing dish bottom flavorings, described ion-exchange chromatography-fluoroscopic examination, detected parameters is set: SCX strong cation exchange chromatography post: column length 250mm, column internal diameter 4.6mm, packing material size 5 μ m; Mobile phase: volume ratio is acetonitrile-0.1% ammonia spirit of 4:6, isocratic elution; Flow velocity: 0.8～1.2mL/min; Column temperature: 30～40 ℃; Sample size: 10～100 μ L; Excitation wavelength: 548～552nm, emission wavelength: 578～582nm, describedly judge that according to liquid chromatogram the criterion whether rhodamine B is arranged in the chafing dish bottom flavorings is: have chromatographic peak to occur if the liquid chromatogram of sample goes out the peak position in rhodamine B standard solution chromatogram, and signal to noise ratio (S/N ratio) is greater than 5, then contain rhodamine B in the judgement sample, if going out the peak position in rhodamine B standard solution chromatogram, the liquid chromatogram of sample do not have chromatographic peak to occur, then do not detect rhodamine B in the sample, the quantitative employing calibration curve method of described rhodamine B is determined.
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| CN102662025B (en) * | 2012-05-22 | 2015-08-26 | 晨光生物科技集团股份有限公司 | The detection method of rhodamine B content in plastic package material |
| CN104034713A (en) * | 2013-03-05 | 2014-09-10 | 厦门大学 | Rapid detection method for Rhodamine B |
| CN105353025A (en) * | 2015-06-19 | 2016-02-24 | 南京工业大学 | Method for rapidly determining rhodamine B in food |
| CN105784453B (en) * | 2016-03-16 | 2018-04-13 | 吉林省水产科学研究院 | The pre-treating method of avermectin and ivermectin residue detection in the flesh of fish |
| CN106290673B (en) * | 2016-09-27 | 2018-05-18 | 深圳市计量质量检测研究院 | A kind of method that eutectic solvent extraction liquid chromatography quickly measures rhodamine B |
| CN110646498A (en) * | 2019-07-08 | 2020-01-03 | 中国检验检疫科学研究院 | Method for rapidly detecting rhodamine B in hotpot condiment and forchlorfenuron in watermelon |
| CN112730644A (en) * | 2020-12-04 | 2021-04-30 | 广东省核工业地质局辐射环境监测中心(广东省铀资源储量评审中心) | Method for determining rhodamine B in chili oil |
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