CN116203115A - ICP-MS (inductively coupled plasma-mass spectrometry) based method for distinguishing green-flavor kiwi fruits from Haiwod kiwi fruits - Google Patents

ICP-MS (inductively coupled plasma-mass spectrometry) based method for distinguishing green-flavor kiwi fruits from Haiwod kiwi fruits Download PDF

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CN116203115A
CN116203115A CN202310006710.4A CN202310006710A CN116203115A CN 116203115 A CN116203115 A CN 116203115A CN 202310006710 A CN202310006710 A CN 202310006710A CN 116203115 A CN116203115 A CN 116203115A
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icp
kiwi fruits
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赵燕妮
燕美如
张俊杰
刘欢
武璇
张坤
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Shaanxi University of Science and Technology
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    • G01—MEASURING; TESTING
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    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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    • G—PHYSICS
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    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40—Concentrating samples
    • G01N1/4022—Concentrating samples by thermal techniques; Phase changes
    • G01N2001/4033—Concentrating samples by thermal techniques; Phase changes sample concentrated on a cold spot, e.g. condensation or distillation

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Abstract

The invention discloses a method for distinguishing green-flavor kiwi fruits from Haiwod kiwi fruits based on ICP-MS elemental analysis. The technical scheme of the invention is as follows: and judging two types of kiwi fruits which are difficult to identify due to similar appearance by utilizing the ratio of the content of magnesium element and the content of chromium element in the kiwi fruits, wherein the kiwi fruits to be detected are green kiwi fruits with the ratio of the content of magnesium element to the content of chromium element of 50 or less, and the kiwi fruits with the content of magnesium element to the content of chromium element of 100 or more are Haiwo kiwi fruits. The invention has the advantages of small sampling amount, short measurement time and accurate and reliable result, and can provide basis for the research of kiwi fruit variety identification.

Description

ICP-MS (inductively coupled plasma-mass spectrometry) based method for distinguishing green-flavor kiwi fruits from Haiwod kiwi fruits
Technical Field
The invention belongs to the field of analytical chemistry, and relates to a method for distinguishing green-flavor kiwi fruits from Haiwo kiwi fruits based on ICP-MS elemental analysis.
Background
Elemental analysis is a chemical analysis method that studies the elemental composition of an organic compound. Currently, methods for elemental analysis mainly include Atomic Absorption Spectroscopy (AAs), atomic Fluorescence Spectroscopy (AFs), inductively coupled plasma mass spectrometry (ICP-Ms), and the like (Zheng Bingzhen, 2017). Inductively coupled plasma-mass spectrometry (ICP-MS) is an analytical method combining ICP technology with mass spectrometry, which can be used for elemental analysis, and can simultaneously determine several tens of trace inorganic elements, including almost all metallic elements and most nonmetallic elements of the periodic table. Compared with the traditional inorganic analysis technology, the ICP-MS has the characteristics of low trace analysis lower limit, small sampling amount, short measurement time and the like, improves the efficiency for the detection and analysis of inorganic elements, extends the monitoring lower limit, and is widely applied to the fields of food, biology, chemical industry, environment, material analysis and the like.
The inductively coupled plasma mass spectrometer has the advantages of inductively coupled plasma and quadrupole mass spectrometer, firstly, an analysis sample is digested, and the analysis sample is prepared into a solution with a certain concentration and then is sent to an atomizer for treatment. The small liquid drops formed through the treatment of the atomizer collide with the inner wall of the atomization chamber to form aerosol fog drops, and plasma is introduced under the action of argon. The plasma atomizes and ionizes the sample at high temperature, and the generated ions are introduced into the vacuum chamber through the interface, and enter the four-level rod mass filter after being focused and deflected by the ion lens. And separating and detecting target ions according to the difference of mass numbers, quantitatively analyzing element mass spectrum peaks, and giving the content of elements contained in the sample to be detected after treatment.
The kiwi fruit is a fruit with rich nutrition, contains rich amino acids and minerals, and has an important function of keeping human health. The Chinese goosebeery planting technology is improved after long-term investigation, breeding and introduction cultivation in China, and the quality of the kiwi fruits is continuously improved. The main species of the kiwi fruits planted in the Shaanxi region at present comprise Xu Xiang, delphinidia chinensis, haiwod, qin Mei and the like. The green fragrance is originally named as 'xi-rhesus 9', the skin is yellow-wool, the pulp is yellow-green, the taste is fresh and sweet, and the green-green-rhesus is inspected by the fruit tree variety inspection committee of Shanxi province in 2008 through more than 10 years of breeding and regional experiments. The kiwi fruit belongs to a delicious kiwi fruit series, and the variety has sweet and sour taste and has the characteristics of strong plant growth vigor, excellent quality, long storage life and the like. The two types of kiwi fruits are similar in appearance, the peel is yellowish green and covered with yellow wool, the pulp is emerald green and the fruit is beautiful, the quality is excellent, the distinction of the two types of kiwi fruits at present depends on the planting experience of fruit farmers and the slight difference of the fluffy and taste of the fruits, and no scientific, efficient, rapid and effective method is available for accurately distinguishing the emerald kiwi fruits from the Haiwod kiwi fruits.
Disclosure of Invention
The invention aims to provide a method for distinguishing green-flavor kiwi fruits from Haiwo kiwi fruits based on ICP-MS element analysis, which utilizes the ratio of the content of magnesium element and the content of chromium element in kiwi fruits to distinguish green-flavor kiwi fruits from Haiwo kiwi fruits.
In order to achieve the above purpose, the technical scheme provided by the invention is as follows:
a method for distinguishing green-flavor kiwi fruits from sea Walder kiwi fruits based on ICP-MS elemental analysis utilizes the ratio of magnesium element and chromium element content in kiwi fruits to distinguish two types of kiwi fruits which are difficult to distinguish due to similar appearance.
Firstly, adopting microwave digestion-inductively coupled plasma mass spectrometry ICP-MS to sequentially analyze a mixed standard solution of magnesium element and chromium element according to the sequence from low concentration to high concentration, and drawing a standard curve; performing ICP-MS analysis on the kiwi fruit sample extracting solution, and determining the content of magnesium element and chromium element in the kiwi fruit sample according to a standard curve; and finally, calculating the ratio of the content of magnesium element to the content of chromium element, wherein the kiwi fruit sample to be detected has the ratio of the content of magnesium element to the content of chromium element of 50 or less, and the kiwi fruit sample to be detected has the ratio of the content of magnesium element to the content of chromium element of 100 or more.
The drawing method of the standard curve comprises the following steps: a mixed standard solution of 5000ug/L magnesium element and 100ug/L chromium element is prepared, then 1% HNO3 is used as a dilution solution, the mixed standard sample is respectively diluted to 50%, 10%, 5%, 1%, 0.5%, 0.1%, 0.05% and 0.01% (V/V), a serial concentration gradient standard solution is obtained, ICP-MS analysis is sequentially carried out, and a standard curve is drawn.
The preparation method of the kiwi fruit sample extracting solution comprises the following steps: pulping kiwi fruit sample, and drying in a freeze dryer to obtain powder; precisely weighing 0.15g of sample powder in a polytetrafluoroethylene digestion tank, adding concentrated nitric acid 6mL, slightly oscillating, uniformly mixing, placing in a microwave digestion instrument, and digesting according to a set digestion program: the power is climbed to 800W for the first 10min, maintained for 5min, and then climbed to 1500W for 15min, and maintained for 30min. After digestion is completed, the digestion solution is cooled to be less than 70 ℃, a small amount of ultrapure water is added for dissolution and transferred into a 100mL volumetric flask for constant volume, so as to obtain a solution to be measured, and 3mL of the solution to be measured is taken.
The detection conditions of the ICP-MS are as follows: the radio frequency power is 1600W, the plasma argon volume flow is 18L/min, the carrier gas volume flow is 0.94L/min, the auxiliary gas volume flow is 1.2L/min, the atomizer type Meinhard, and the residence time is 50ms; the test was performed using a collision mode Kenetic Energy Discrimination (KED) with a helium flow set to 3.7mL/min.
The main technical indexes of instrument tuning are as follows: routine analysis sensitivity index 115 In＞40000 cps， 238 U＞30000 cps， 9 Be > 2000 cps; background: bkgd220 is less than or equal to 1 cps, and the ratio of cerium element oxide to cerium element 156 CeO + / 140 Ce + : less than or equal to 2.5 percent, the ratio of the double charge and single charge ion of cerium element 70 Ce 2+ / 140 Ce + : the mass number and the resolution are within the range of 0.65-0.8U at the peak height of 10% of Li, mg, in and U. Before the instrument test, the rectangular tube position, the atomizer flow, the quadrupole ion deflector voltage and the detector voltage are optimized, and the detector dual mode correction is performed.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, the ratio of the content of magnesium element and the content of chromium element in the kiwi fruit sample and the correlation of sample types are utilized to judge two types of kiwi fruit varieties which are difficult to distinguish due to similar appearance. The invention has the following characteristics: high sensitivity, small sampling amount, short measurement time and accurate and reliable result. The method can provide reference for kiwi fruit variety discrimination research.
Drawings
FIG. 1 is a graph showing the ratio of the content of magnesium element to the content of chromium element in the examples.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but embodiments of the present invention include, but are not limited to, the scope of the following examples.
A method for distinguishing green-flavor kiwi fruits from sea Walder kiwi fruits based on ICP-MS elemental analysis utilizes the ratio of magnesium element and chromium element content in kiwi fruits to distinguish two types of kiwi fruits which are difficult to distinguish due to similar appearance. The kiwi fruit sample to be detected is a green-flavor kiwi fruit sample with the ratio of magnesium element to chromium element content of 50 or below and the kiwi fruit sample to be detected is a Haiwo kiwi fruit sample with the ratio of magnesium element to chromium element content of 100 or above.
The specific method comprises the following steps:
firstly, adopting microwave digestion-inductively coupled plasma mass spectrometry ICP-MS to sequentially analyze a mixed standard solution of magnesium element and chromium element according to the sequence from low concentration to high concentration, and drawing a standard curve; performing ICP-MS analysis on the kiwi fruit sample extracting solution, and determining the content of magnesium element and chromium element in the kiwi fruit sample according to a standard curve; and finally calculating the ratio of the content of magnesium element to the content of chromium element.
The samples to be tested comprise 5 green Chinese goosebeery fruits, which are respectively numbered CX-1, CX-2, CX-3, CX-4 and CX-5; the number of the Haiwo kiwi fruit samples is 4, and the HWD samples are respectively numbered as HWD-1, HWD-2, HWD-3 and HWD-4.
The drawing method of the standard curve comprises the following steps: preparing a mixed standard solution of 5000ug/L magnesium element and 100ug/L chromium element, and then using 1% HNO 3 As a dilution solution, the mixed standard was diluted to 50%, 10%, 5%, 1%, 0.5%, 0.1%, 0.05%, 0.01% (V/V), respectively, to obtain standard solutions of a series of concentration gradients, and ICP-MS analysis was performed sequentially, and a standard curve was drawn.
The preparation method of the kiwi fruit sample extracting solution comprises the following steps: pulping kiwi fruit sample, and drying in a freeze dryer to obtain powder; precisely weighing 0.15g of sample powder in a polytetrafluoroethylene digestion tank, adding 6mL of concentrated nitric acid, slightly oscillating, uniformly mixing, placing in a microwave digestion instrument, and digesting according to a set digestion program: the power of 800W climbs for the first 10min, is maintained for 5min, and then the power of 1500W climbs for 15min, and is maintained for 30min. After digestion is completed, the digestion solution is cooled to be less than 70 ℃, a small amount of pure water is added for dissolution, and the solution is transferred into a 100mL measuring flask for constant volume, so as to obtain the solution to be measured.
The detection conditions of the ICP-MS are as follows: the radio frequency power is 1600W, the plasma argon volume flow is 18L/min, the carrier gas volume flow is 0.94L/min, the auxiliary gas volume flow is 1.2L/min, the atomizer type Meinhard is adopted, and the residence time is 50ms; the main technical indexes of instrument tuning are as follows: conventional analytical sensitivity index 115In > 40000cps,238U > 30000cps,9Be > 2000 cps; the collision mode was Kenetic Energy Discrimination (KED) and the helium volumetric flow was 3.7mL/min.
The contents of magnesium and chromium in the kiwi fruits are obtained under the analysis condition, and the ratio of the contents of the magnesium and the chromium is found to be obviously changed, and the ratio is shown in a table 1.
Table 1 Experimental material information and ratio of magnesium element to chromium element content used in examples
Figure 124417DEST_PATH_IMAGE002
The invention takes the ratio of magnesium element and chromium element content as the standard for distinguishing the green-flavor kiwi fruits from the Haiwod kiwi fruits. The kiwi fruit sample to be detected is a green-flavor kiwi fruit sample with the ratio of magnesium element to chromium element content of 50 or below and the kiwi fruit sample to be detected is a Haiwo kiwi fruit sample with the ratio of magnesium element to chromium element content of 100 or above.

Claims (6)

1. The method for distinguishing the green-flavor kiwi fruits from the Haiwod kiwi fruits based on ICP-MS elemental analysis is characterized by comprising the following steps of:
and analyzing the green Chinese goosebeery and the Haiwod Chinese goosebeery by adopting microwave digestion-inductively coupled plasma mass spectrometry ICP-MS to obtain the content of magnesium element and chromium element, and distinguishing the two types of Chinese goosebeery varieties which are difficult to distinguish due to similar appearance by utilizing the ratio of the content of magnesium element to the content of chromium element in the Chinese goosebeery fruits.
2. The method for distinguishing between green and sea kiwi fruits based on ICP-MS elemental analysis according to claim 1, wherein:
the method for distinguishing the green-flavor kiwi fruits and the Haiwod kiwi fruits specifically comprises the following steps:
firstly, adopting microwave digestion-inductively coupled plasma mass spectrometry ICP-MS to sequentially analyze a mixed standard solution of magnesium element and chromium element according to the sequence from low concentration to high concentration, and drawing a standard curve; performing ICP-MS analysis on the kiwi fruit sample extracting solution, and determining the content of magnesium element and chromium element in the kiwi fruit sample according to a standard curve; and finally, calculating the ratio of the content of magnesium element to the content of chromium element, wherein the kiwi fruit sample to be detected has the ratio of the content of magnesium element to the content of chromium element of 50 or less, and the kiwi fruit sample to be detected has the ratio of the content of magnesium element to the content of chromium element of 100 or more.
3. The method for distinguishing between green and sea kiwi fruits based on ICP-MS elemental analysis according to claim 2, wherein:
the drawing method of the standard curve comprises the following steps: preparing a mixed standard solution of 5000ug/L magnesium element and 100ug/L chromium element, and then using 1% HNO 3 As a dilution solution, the mixed standard was diluted to 50%, 10%, 5%, 1%, 0.5%, 0.1%, 0.05%, 0.01% (V/V), respectively, to obtain standard solutions of a series of concentration gradients, and ICP-MS analysis was performed sequentially, and a standard curve was drawn.
4. A method for distinguishing green-flavor kiwi fruits from sea-bodied kiwi fruits based on ICP-MS elemental analysis according to claim 3, wherein:
the preparation method of the kiwi fruit sample extracting solution comprises the following steps:
pulping kiwi fruit sample, and drying in a freeze dryer to obtain powder; precisely weighing 0.15g of sample powder in a polytetrafluoroethylene digestion tank, adding concentrated nitric acid 6mL, slightly oscillating, uniformly mixing, placing in a microwave digestion instrument, and digesting according to a set digestion program: performing power climbing to 800W for the first 10min, maintaining for 5min, performing power climbing to 1500W for 15min, and maintaining for 30 min; after digestion is completed, the digestion solution is cooled to be less than 70 ℃, a small amount of ultrapure water is added for dissolution and transferred into a 100mL volumetric flask for constant volume, so as to obtain a solution to be measured, and 3mL of the solution to be measured is taken.
5. The method for distinguishing between green and sea kiwi fruits based on ICP-MS elemental analysis according to claim 4, wherein:
the detection conditions of the ICP-MS are as follows: the radio frequency power is 1600W, the plasma argon volume flow is 18L/min, the carrier gas volume flow is 0.94L/min, the auxiliary gas volume flow is 1.2L/min, the atomizer type Meinhard, and the residence time is 50ms; the test was performed using collision mode kenetic energy discrimination with a helium flow set to 3.7mL/min.
6. The method for distinguishing between green and sea kiwi fruits based on ICP-MS elemental analysis according to claim 5, wherein:
the main technical indexes of instrument tuning are as follows: routine analysis sensitivity index 115 In＞40000 cps， 238 U＞30000 cps， 9 Be > 2000 cps; background: bkgd220 is less than or equal to 1 cps, and the ratio of cerium element oxide to cerium element 156 CeO + / 140 Ce + : less than or equal to 2.5 percent, the ratio of the double charge and single charge ion of cerium element 70 Ce 2+ / 140 Ce + : the mass number and the resolution are within the range of 0.65-0.8U at the peak height of 10% of Li, mg, in and U; before the instrument test, the rectangular tube position, the atomizer flow, the quadrupole ion deflector voltage and the detector voltage are optimized, and the detector dual mode correction is performed.
CN202310006710.4A 2023-01-04 2023-01-04 ICP-MS (inductively coupled plasma-mass spectrometry) based method for distinguishing green-flavor kiwi fruits from Haiwod kiwi fruits Pending CN116203115A (en)

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