CN111307927A - Rapid screening method for abnormal elements in white spirit - Google Patents
Rapid screening method for abnormal elements in white spirit Download PDFInfo
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- CN111307927A CN111307927A CN202010204147.8A CN202010204147A CN111307927A CN 111307927 A CN111307927 A CN 111307927A CN 202010204147 A CN202010204147 A CN 202010204147A CN 111307927 A CN111307927 A CN 111307927A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
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- G—PHYSICS
- 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
- G01N1/44—Sample treatment involving radiation, e.g. heat
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Abstract
The invention discloses a method for rapidly screening abnormal elements in white spirit, which belongs to the technical field of chemical analysis and detection and comprises the following steps: and respectively carrying out full-scan detection on the standard wine sample and the abnormal wine sample by adopting ICP-MS, and comparing two ICP-MS spectrograms to judge abnormal elements in the abnormal wine sample. The screening of the method of the invention completely avoids the pollution risk of elements in the white spirit, and is particularly suitable for searching reasons of abnormal white spirit (turbidity, precipitation, obvious color, peculiar smell and the like) so as to control the quality of the white spirit.
Description
Technical Field
The invention belongs to the technical field of chemical analysis and detection, and particularly relates to a rapid screening method for abnormal elements in white spirit.
Background
The white spirit is obtained by fermenting and distilling one or more grains, and various trace elements are possibly introduced in various production links and influence the quality of the white spirit in a non-negligible way. On one hand, the heavy metals of lead Pb, manganese Mn, cadmium Cd, arsenic As, barium Ba and the like directly influence the human health, wherein the lead Pb content is listed As a national standard health index of the white spirit. On the other hand, the content ratio of various elements also directly influences the sensory quality of the white spirit: the appropriate amount of metal elements can reduce the irritation of the wine, make the wine taste soft and improve the quality of the white spirit; improper amount of metal elements can cause the liquor to have peculiar smells such as salty, bitter, astringent and iron fishy smell, or cause the liquor to be colored (such as iron Fe, manganese Mn and the like) and turbid precipitates (such as calcium Ca, magnesium Mg, barium Ba and the like) to reduce the quality of the liquor. Therefore, the screening of various elements is an essential important link for the control of the quality of the white spirit.
Inductively coupled plasma mass spectrometry (ICP-MS) is an analytical technique that combines ICP and MS together. In the ICP-MS, ICP is an ion source, high-temperature plasma is formed inside a coil by using a high-power high-frequency radio-frequency signal applied to an inductive coil, and the balance and continuous ionization of the plasma are ensured by using the pushing of gas; the high-temperature plasma ionizes elements in most samples to generate an electron, so that monovalent positive ions are formed; MS is a "mass screening, analyzer" that measures the intensity of an ion by selecting ions of different mass-to-nuclear ratios (m/z) and then analyzes and calculates the intensity of an element.
Disclosure of Invention
The invention aims to provide a method for rapidly screening abnormal elements in white spirit, which completely avoids the pollution risk of the elements in the white spirit through screening by the method, and is particularly suitable for searching reasons of the abnormal white spirit (turbidity, precipitation, obvious color, peculiar smell and the like) so as to control the quality of the white spirit leaving factory.
The invention provides a method for rapidly screening abnormal elements in white spirit, which comprises the following steps: respectively carrying out full-scan detection on the standard wine sample and the abnormal wine sample by adopting ICP-MS, and comparing two ICP-MS spectrograms to judge abnormal elements in the abnormal wine sample;
the detection condition of the ICP-MS is one of the following two modes:
CCT collision cell mode: scanning mode: full scanning; forward power: 1300-1350W; sampling depth: 100 to 195 step; cooling air flow: 12.5-15.5L/min; auxiliary air flow rate: 0.67-1.15L/min; flow rate of atomizing gas: 0.80-1.00L/min; CCT collision gas composition: 7% H293% He; CCT collision air flow rate: 5.3-6 ml/min; rotation speed of peristaltic pump: 30 r/min;
standard mode: the scanning mode is as follows: full scanning; forward power: 1250-1350W; sampling depth: 100 to 210 step; cooling air flow: 12.5-15.5L/min; auxiliary air flow rate: 0.67-1.15L/min; flow rate of atomizing gas: 0.80-1.00L/min; rotation speed of peristaltic pump: 30 r/min.
According to the method for rapidly screening the abnormal elements in the white spirit, the wine sample needs to be pretreated before detection, and the pretreatment mode is water bath evaporation or microwave digestion.
According to the rapid screening method for the abnormal elements in the white spirit, 5-10 mL of white spirit is put into a beaker in a water bath kettle, ethanol is volatilized at 62-67 ℃ in the water bath kettle, the white spirit is steamed until only 0.4-0.6 mL of liquid remains in the beaker, the white spirit is diluted with 3-6 mL of 1% nitric acid solution and shaken uniformly and then transferred into a 50mL volumetric flask, then the plastic beaker is washed with 1% nitric acid solution for 3-5 times, the washing liquid is transferred into the volumetric flask, and finally the volume is fixed to 50mL by using 1% nitric acid solution.
According to the rapid screening method for the abnormal elements in the white spirit, 5-10 mL of white spirit is taken, ethanol is volatilized to 2-4 mL under the condition that the temperature of the white spirit is lower than 65 ℃ on an acid dispelling device, 5-6 mL of nitric acid is added, the mixture is placed for 1h, then is digested by a microwave digestion instrument, is taken out after cooling, is placed on the acid dispelling device to be heated for 50min under the condition that the temperature of the white spirit is lower than 65 ℃, is made to be 25mL with water, and is uniformly mixed to obtain the special white spirit.
According to the rapid screening method for abnormal elements in the white spirit, the digestion program of the microwave digestion instrument is as follows: heating to 120 ℃ at the speed of 10-15 ℃/min, and keeping for 8-10 min; heating to 150 ℃ at the speed of 3-5 ℃/min, and keeping for 15-20 min; and finally, heating to 180 ℃ at the speed of 3-5 ℃/min, and keeping for 30 min.
According to the method for rapidly screening the abnormal elements in the white spirit, the standard wine sample is qualified finished wine of the abnormal wine sample brand over the years.
Compared with the prior art, the invention has the beneficial effects that:
aiming at the abnormal elements in the unknown sample (such as turbidity, precipitation and discoloration in white wine), the method can quickly and uninterruptedly screen the abnormal sample and compare ICP-MS full-scan spectrograms of the two samples by scanning the elements in the abnormal sample and the treatment liquid of the wine sample qualified in the same brand in the past year, thereby playing an important guiding role in searching abnormal causes.
Drawings
FIG. 1 is a mass spectrum M/Z20-60 of 3 years-old qualified samples of a certain brand of white spirit;
FIG. 2 is a mass spectrum M/Z50-210 of 3 years-old qualified samples of a certain brand of white spirit;
FIG. 3 is a mass spectrum M/Z20-60 of an abnormal taste wine sample and a qualified wine sample of the same brand over years;
FIG. 4 is a mass spectrum M/Z50-210 of an abnormal taste wine sample and a qualified wine sample of the same brand over years;
FIG. 5 is a mass spectrum M/Z20-60 of a slightly cloudy wine sample 1 and a wine sample qualified in the same brand according to years;
FIG. 6 is a mass spectrum M/Z60-210 of a slightly cloudy wine sample 1 and a qualified wine sample of the same brand over the years;
FIG. 7M/Z0-210 mass spectrum of slightly cloudy wine sample 2 versus a calendar year acceptable wine sample of the same brand.
Detailed Description
The invention provides a method for rapidly screening abnormal elements in white spirit, which comprises the following steps: respectively carrying out full-scan detection on the standard wine sample and the abnormal wine sample by adopting ICP-MS, and comparing two ICP-MS spectrograms to judge abnormal elements in the abnormal wine sample;
the detection condition of the ICP-MS is one of the following two modes:
CCT collision cell mode: scanning mode: full scanning; forward power: 1300-1350W; sampling depth: 100 to 195 step; cooling air flow: 12.5-15.5L/min; auxiliary air flow rate: 0.67-1.15L/min; flow rate of atomizing gas: 0.80-1.00L/min; CCT collision gas composition: 7% H2, 93% He; CCT collision air flow rate: 5.3-6 ml/min; rotation speed of peristaltic pump: 30 r/min;
standard mode: the scanning mode is as follows: full scanning; forward power: 1250-1350W; sampling depth: 100 to 210 step; cooling air flow: 12.5-15.5L/min; auxiliary air flow rate: 0.67-1.15L/min; flow rate of atomizing gas: 0.80-1.00L/min; rotation speed of peristaltic pump: 30 r/min.
The CCT collision pool mode is suitable for element conventional scanning screening, but the scanning screening is preferably carried out by adopting a standard mode under the condition of low element concentration.
The method of the invention can rapidly screen out abnormal elements in abnormal wine samples, and the types of the abnormal elements comprise: metals Li, Be, Na, Mg, Al, K, Ca, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, Ge, Rb, Sr, Y, Zr, Nb, Mo, Tc, Ru, Rh, Pd, Ag, Cd, In, Sn, Sb, Cs, Ba, Hf, Ta, W, Re, Os, Ir, Pt, Au, Hg, Tl, Pb, Bi, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Th, U, Np, Pu; nonmetal B, Si, P, S, Cl, As, Se, Br, Te and I, short detection time and wide detection range, almost covers all element types (except short half-life elements) in the nature, and only 26 elements can be measured by adopting peak jump scanning compared with national standard 'measurement of multiple elements in food', and the analysis index number of the method is far greater than that of national (enterprise) standards.
Because the samples used in the embodiment of the invention are all real finished wine, and some elements (such as M/Z78 Se, 89Y, 121Sb, 139La and the like) in the wine are difficult to observe in the range of measurement range in the attached drawing of the invention due to low ionic strength, and can be observed on an instrument software drawing by adjusting the measurement range of the ordinate axis at any time in actual operation. A drawing herein is divided into M/Z50-210 and M/Z20-60 to facilitate viewing of various elements that are not in one range.
The wine sample is pretreated before detection, and the pretreatment mode is water bath evaporation or microwave digestion.
The water bath evaporation is to take 5-10 mL of white spirit into a beaker, volatilize ethanol at 62-67 ℃ in a water bath kettle, evaporate until only 0.4-0.6 mL of liquid remains in the beaker, dilute and shake 3-6 mL of 1% nitric acid solution, carefully transfer the beaker into a 50mL volumetric flask, wash the plastic beaker 3-5 times with 1% nitric acid solution, transfer the washing solution into the volumetric flask, and finally fix the volume to 50mL with 1% nitric acid solution;
the microwave digestion is to take 5-10 mL of white spirit, volatilize ethanol to 2-4 mL under the condition of less than 65 ℃ on an acid expeller, add 5-6 mL of nitric acid, stand for 1h, digest by using a microwave digestion instrument, cool and take out, then place on the acid expeller to heat for 50min under the condition of less than 65 ℃, fix the volume to 25mL by using water, and mix uniformly to obtain the product.
The digestion program of the microwave digestion instrument is as follows: heating to 120 ℃ at the speed of 10-15 ℃/min, and keeping for 8-10 min; heating to 150 ℃ at the speed of 3-5 ℃/min, and keeping for 15-20 min; and finally, heating to 180 ℃ at the speed of 3-5 ℃/min, and keeping for 30 min.
The following examples are provided to further illustrate the embodiments of the present invention and are not intended to limit the scope of the present invention.
The main instruments used in the examples: x-series2 inductively coupled plasma mass spectrometer, Thermo corporation, USA; CEM corporation, MARS 6 microwave digestion instrument; a water bath kettle.
Example 1 detection of multiple elements in a sample of a certain brand of Baijiu that is acceptable over a period of years
Standard wine sample: 3 liquor samples (different batches of finished liquor) qualified for a certain brand of white liquor in the past year are all 52% vol.
Pretreatment (microwave digestion method): taking a 10mL white spirit uniform wine sample, volatilizing to 4mL in an acid expeller at 65 ℃, adding 6mL nitric acid, covering and placing for 1h, screwing a tank cover, digesting according to the standard operation steps of a microwave digestion instrument, cooling, slowly opening the tank cover to exhaust, flushing an inner cover with a small amount of water, placing the digestion tank on the acid expeller, heating for 50min at 65 ℃, adding water to reach a constant volume of 25mL, and mixing uniformly to obtain a white spirit treatment solution. At this time, the content of the wine-like organic matter should be less than 4%. The digestion program of the microwave digestion instrument is as follows: heating to 120 deg.C at a rate of 15 deg.C/min, and maintaining for 8 min; heating to 150 deg.C at a rate of 5 deg.C/min, and maintaining for 15 min; finally, the temperature is increased to 180 ℃ at the speed of 5 ℃/min and is kept for 30 min.
Detection conditions for ICP-MS (CCT collision cell mode): the scanning mode is as follows: full scanning; forward power: 1320W; sampling depth: 187 step; cooling air flow: 13.0L/min; auxiliary air flow rate: 0.80L/min; flow rate of atomizing gas: 0.88L/min; CCT collision gas composition: 7% H293% He; CCT collision air flow rate: 5.95 ml/min; rotation speed of peristaltic pump: 30 r/min.
The ICP-MS was used to test the various elements in the above samples under full scan conditions, and the results are shown in fig. 1 and fig. 2.
Fig. 1 and fig. 2 show that the peak heights of all elements of the ICP-MS full scan images of 3 wine samples qualified over the years are substantially consistent, which indicates that the types and contents of all elements in the brand of white spirit are stable throughout the year after the normal production process.
Example 2 detection of multiple elements in an abnormal tasting wine sample
Abnormal wine sample: 52% vol wine-like, the mouthfeel is abnormal.
Standard wine sample: abnormal taste wine samples of 2 wine samples (different batches of finished wine) which are qualified in the same brand of white spirit over the years are all 52% vol.
Pretreatment: the wine sample was pretreated by the microwave digestion method in example 1.
Detection conditions for ICP-MS (CCT collision cell mode): the scanning mode is as follows: full scanning; forward power: 1320W; sampling depth: 187 step; cooling air flow: 13.0L/min; auxiliary air flow rate: 0.80L/min; flow rate of atomizing gas: 0.88L/min; CCT collision gas composition: 7% H293% He; CCT collision air flow rate: 5.95 ml/min; rotation speed of peristaltic pump: 30 r/min.
The ICP-MS is adopted to test various elements in the abnormal wine sample under the full scanning state, and the results are shown in the figure 3 and the figure 4.
Observing the abnormal taste wine sample atlas (figure 3 and figure 4), wherein the normal element amount is the result of the wine sample qualified in the same brand all the year round, the abnormal element amount is the result of the abnormal taste wine sample, and the index peaks of Mg, K, Ca, Fe, Mn, Cu, Zn, Sr and the like in the abnormal taste wine sample are found to be obviously higher than those of the standard wine sample, which shows that the abnormal content of part of metal elements in the abnormal taste wine sample causes the incoordination of the taste of the white spirit, and the production process needs to be checked by a winery based on the abnormal content. The results show that the method is feasible to screen abnormal elements in the white spirit (compared with the liquor samples qualified in the past year).
Example 3 detection of multiple elements in slightly cloudy wine sample 1
Abnormal wine sample: slightly hazy wine-like 1, 52% vol.
Standard wine sample: slightly cloudy wine sample 1 and 2 wine samples (different batches of finished wine) which are qualified in the same brand of white wine in the past year are all 52% vol.
Pretreatment (water bath evaporation): taking 10ml of even white spirit sample into a plastic baked cake, volatilizing ethanol at 65 ℃ in a water bath, steaming until about 0.5ml of liquid is left in a plastic beaker, diluting with 5ml of nitric acid solution (1%), shaking uniformly, carefully transferring into a 50ml volumetric flask, washing the plastic beaker with the nitric acid solution for 4 times, transferring the washing liquid into the volumetric flask, and finally fixing the volume to 50ml with the nitric acid solution.
Detection conditions for ICP-MS (CCT collision cell mode): the scanning mode is as follows: full scanning; forward power: 1320W; sampling depth: 187 step; cooling air flow: 13.0L/min; auxiliary air flow rate: 0.80L/min; flow rate of atomizing gas: 0.88L/min; CCT collision gas composition: 7% H293% He; CCT collision air flow rate: 5.95 ml/min; rotation speed of peristaltic pump: 30 r/min. .
ICP-MS is adopted to test various elements in the wine sample under the full scanning state, and the results are shown in figure 5 and figure 6.
And observing the spectrum (figure 5 and figure 6) of the slightly turbid wine sample 1, wherein the normal amount of elements is the result of the wine sample qualified in the same brand in the years, and the abnormal amount of elements is the result of the slightly turbid wine sample 1, and the index peaks of Fe, Sn, Ba and the like in the slightly turbid wine sample 1 are obviously higher than those of the standard wine sample, which shows that the slight turbidity of the white spirit is caused by the abnormal content (particularly the abnormal content of Ba) of part of the metal elements in the abnormal wine sample 1. The above results again demonstrate that the method of the present invention is feasible to screen for abnormal elements in white spirit (compared with the liquor samples qualified in the past years).
Example 4 detection of multiple elements in slightly cloudy wine sample 2
Abnormal wine sample: slightly hazy wine-like 2, 52% vol.
Standard wine sample: the slightly turbid liquor sample 2 is 2 liquor samples (different batches of finished liquor) qualified in the same brand of white liquor in the past year, and the liquor samples are all 52% vol.
Pretreatment (water bath evaporation): the above-mentioned wine sample was pretreated by the water-bath evaporation method in example 3
Detection conditions for ICP-MS (Standard mode): the scanning mode is as follows: full scanning; forward power: 1320W; sampling depth: 187 step; cooling air flow: 13.0L/min; auxiliary air flow rate: 0.80L/min; flow rate of atomizing gas: 0.88L/min; rotation speed of peristaltic pump: 30 r/min.
The above wine samples were tested for various elements using ICP-MS under full scan conditions and the results are shown in figure 7.
The spectrum of the slightly turbid wine sample 2 (figure 7) is observed, the normal amount of elements is the result of the wine sample qualified in the same brand in years, the abnormal amount of elements is the result of the slightly turbid wine sample 2, similar to the result of the example 3, the index peaks of Sn, Ba and the like in the slightly turbid wine sample 2 are obviously higher than those of the standard wine sample, and the abnormal condition of the wine sample is probably caused by the abnormal content of the elements of Sn, Ba and the like (particularly the abnormal content of Ba). The above results again demonstrate that the method of the present invention is feasible to screen for abnormal elements in white spirit (compared with the liquor samples qualified in the past years).
Claims (6)
1. The method for rapidly screening abnormal elements in white spirit is characterized by comprising the following steps: respectively carrying out full-scan detection on the standard wine sample and the abnormal wine sample by adopting ICP-MS, and comparing two ICP-MS spectrograms to judge abnormal elements in the abnormal wine sample;
the detection condition of the ICP-MS is one of the following two modes:
CCT collision cell mode: scanning mode: full scanning; forward power: 1300-1350W; sampling depth: 100 to 195 step; cooling air flow: 12.5-15.5L/min; auxiliary air flow rate: 0.67-1.15L/min; flow rate of atomizing gas: 0.80-1.00L/min; CCT collision gas composition: 7% H293% He; CCT collision air flow rate: 5.3-6 ml/min;rotation speed of peristaltic pump: 30 r/min;
standard mode: the scanning mode is as follows: full scanning; forward power: 1250-1350W; sampling depth: 100 to 210 step; cooling air flow: 12.5-15.5L/min; auxiliary air flow rate: 0.67-1.15L/min; flow rate of atomizing gas: 0.80-1.00L/min; rotation speed of peristaltic pump: 30 r/min.
2. The method for rapidly screening abnormal elements in white spirit according to claim 1, which is characterized in that: the wine sample needs to be pretreated before detection, and the pretreatment mode is water bath evaporation or microwave digestion.
3. The method for rapidly screening abnormal elements in white spirit according to claim 2, which is characterized in that: and in the water bath evaporation, 5-10 mL of white spirit is taken into a beaker, ethanol is volatilized at 62-67 ℃ in a water bath kettle, the white spirit is evaporated until only 0.4-0.6 mL of liquid is left in the beaker, the white spirit is diluted by 3-6 mL of 1% nitric acid solution and shaken uniformly and then transferred into a 50mL volumetric flask, the plastic beaker is washed by 3-5 times by using the 1% nitric acid solution, the washing liquid is transferred into the volumetric flask, and finally the volume is fixed to 50mL by using the 1% nitric acid solution.
4. The method for rapidly screening abnormal elements in white spirit according to claim 2, which is characterized in that: the microwave digestion is to take 5-10 mL of white spirit, volatilize ethanol to 2-4 mL under the condition of less than 65 ℃ on an acid expeller, add 5-6 mL of nitric acid, stand for 1h, digest by using a microwave digestion instrument, cool and take out, then place on the acid expeller to heat for 50min under the condition of less than 65 ℃, fix the volume to 25mL by using water, and mix uniformly to obtain the product.
5. The method for rapidly screening abnormal elements in white spirit according to claim 4, which is characterized in that: the digestion program of the microwave digestion instrument is as follows: heating to 120 ℃ at the speed of 10-15 ℃/min, and keeping for 8-10 min; heating to 150 ℃ at the speed of 3-5 ℃/min, and keeping for 15-20 min; and finally, heating to 180 ℃ at the speed of 3-5 ℃/min, and keeping for 30 min.
6. The method for rapidly screening abnormal elements in white spirit according to any one of claims 1 to 5, which is characterized by comprising the following steps: the standard wine sample is qualified finished wine of abnormal wine sample brands all the year round.
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