CN101477053B - Measuring method for inorganic cobalt content in biological chemical, food and feed - Google Patents
Measuring method for inorganic cobalt content in biological chemical, food and feed Download PDFInfo
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- CN101477053B CN101477053B CN2008102467361A CN200810246736A CN101477053B CN 101477053 B CN101477053 B CN 101477053B CN 2008102467361 A CN2008102467361 A CN 2008102467361A CN 200810246736 A CN200810246736 A CN 200810246736A CN 101477053 B CN101477053 B CN 101477053B
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Abstract
The invention relates to a method for determining inorganic cobalt in biological chemicals, food and feedstuff through an inductively coupled plasma atomic emission spectrometer. 2 percent of a hydrochloric acid water solution and 12 percent of the hydrochloric acid water solution are added into samples to be tested; the inorganic cobalt is extracted in a form of chloride under dilute hydrochloric acid conditions after water bath and oscillation leaching; and then the inductively coupled plasma atomic emission spectrometer is used for determining a sample treatment liquid. The detection of the content of the inorganic cobalt in the biological chemicals, the food and the feedstuff by the method is quick and effective, and the relative average deviation is less than 5 percent; therefore, the method provides a reliable method with reliable and convenient implementation for detecting the content of the inorganic cobalt in the biological chemicals, the food and the feedstuff, and can meet the requirement in the research and production.
Description
Technical field
The present invention relates to a kind of assay method, particularly relate to a kind of method that inorganic cobalt content in biochemicals, food, the feed is detected by inductively coupled plasma atomic emission spectrometer inorganic cobalt in biochemicals, food, the feed.
Background technology
Cobalt can exist with different chemical specieses, comprises organic cobalt and inorganic cobalt, and inorganic cobalt is the cobalt total amount that exists with the inorganic cobalt compound form.International cancer tissue (IARC) is classified cobalt and compound thereof as suspicious human carcinogenic substance.The same with other trace element, cobalt is excessive in animal feed, Chinese medicine and human foods, then might suppress the growth of body, even causes serious intoxication accident.The toxic action of cobalt mainly shows as polycythemia, goitre, cardiomyopathy and pancreas, nervous system damage.Inorganic cobalt in the food can absorb in the small intestine running, discharges from urine, ight soil, sweat and hair.Inorganic cobalt is attached on the albumin in blood plasma, and it is stored in liver and kidney at first, is stored in bone, spleen, pancreas, small intestine and its hetero-organization then.The inorganic cobalt compound as: cobalt chloride or cobalt sulfide Excessive Intake have carcinogenesis.Because the difference of bion factor, cobalt nutrient concentration and toxic concentration in body exist huge difference, there is not good check and analysis method for inorganic cobalt at present, therefore the utmost point is necessary to set up a kind of quick, accurate, convenient and economic detection method, help monitoring the use amount that contains of inorganic cobalt in biochemicals, food, the feed, thereby ensure health and herding safety.
Summary of the invention
Technical matters to be solved by this invention is, overcome the technical difficult point of pre-treatment lixiviate inorganic cobalt, by groping the best proportioning of hydrochloric acid solution, best extraction time and best instrument condition and a kind of assay method to inorganic cobalt in biochemicals, food, the feed is provided.
For achieving the above object, the present invention takes following design proposal:
A kind of assay method to inorganic cobalt in biochemicals, food, the feed that the present invention relates to comprises the steps:
Solid sample is through crossing 80 mesh sieves after the drying and crushing, the bright sample of animal tissue breaks into homogenate.
Take by weighing the sample 5g～10g of animal tissue of the solid sample that sieves or bright sample making beating, place 25ml tool plug scale color comparison tube, add 12% aqueous hydrochloric acid solution to the scale mixing, place 90 ℃ water-bath 4 hours～8 hours, failure of oscillation does not swing therebetween, makes the abundant lixiviate of sample, takes out and cools off with 0.45 μ m membrane filtration, blank assay is made in the machine test simultaneously on the filtrate.
Fluid sample takes by weighing 0.5g～10g, places 25ml tool plug scale color comparison tube, adds 2% aqueous hydrochloric acid solution to the scale mixing, and vibration is 15 minutes under room temperature, leaves standstill the back as if the not muddy supernatant of then getting of leaching liquor, last machine test; If the leaching liquor muddiness places 60 ℃ of water-baths 15 minutes, use 0.45 μ m membrane filtration again, blank assay is made in the machine test simultaneously on the filtrate.
Press concentration gradient order from low to high with inductively coupled plasma atomic emission spectrometer, measure the spectral emissions intensity of object element in the serial solution of calibration, concentration with calibration solution is horizontal ordinate, is that ordinate is drawn calibration curve with the signal intensity of element to be measured.Calibration curve detects blank solution and sample treatment solution after setting up.
Result of calculation, the computing formula of inorganic cobalt is in the sample:
The content of inorganic cobalt in the X-sample, unit are every kilogram (mg/kg) of milligram;
C
0-blank solution concentration, unit is every liter (mg/l) of milligram;
C
1-sample solution concentration, unit is every liter (mg/l) of milligram;
V-constant volume, unit are milliliter (ml);
F-sample solution extension rate;
The m-sample quality, unit is gram (g).
Preferably, solid sample quality 5g～10g adds 12% aqueous hydrochloric acid solution to 25ml color comparison tube constant volume; Fluid sample quality 0.5g～10g, the aqueous hydrochloric acid solution of adding 2% is to 25ml color comparison tube constant volume.
Preferably, vibration is 4 hours～8 hours under the water bath condition that solid sample is 90 ℃, and the fluid sample room temperature condition is vibration 15 minutes and 60 ℃ of water-baths 15 minutes when muddy down.
The described condition of utilizing inductively coupled plasma atomic emission spectrometer to detect is:
Incident power: 1150W;
Atomization gas pressure: 0.18Mpa;
Secondary air amount: 0.5L/min;
Observed altitude: 8mm;
Pump speed: 50rpm;
And according to the typical curve standard measure.
Advantage of the present invention is: adopt inorganic cobalt content in method detection of biological chemicals of the present invention, food, the feed, and accurate and effective, RSD detects and is limited to 0.01mg/kg less than 5%, and concentration limit is 0.002mg/l.This shows that method of the present invention is the content of inorganic cobalt in detection of biological chemicals, food, the feed, a kind of method of implementing be convenient to reliably be provided, can satisfy research and produce in needs.
Embodiment
Embodiment 1, and the precision of inorganic cobalt content and the recovery detect in animal tissue's sample:
The bright sample making beating of animal tissue's sample takes by weighing 5.0015g, and (accurately weighing to 0.0001 gram) in 25ml tool plug scale color comparison tube, adds 12% aqueous hydrochloric acid solution to the scale mixing.Place 90 ℃ water-bath 4 hours～8 hours, failure of oscillation does not swing therebetween, makes the abundant lixiviate of sample, takes out cooling with 0.45 μ m membrane filtration, and machine is tested on the filtrate, makes blank assay simultaneously.
Use the Co standard reserving solution: single element solution composition analytical standard material cobalt, 1000mg/L, medium 5%HCl; Preparation Co working solution, concentration gradient 0.0mg/L, 0.01mg/L, 0.05mg/L, 0.1mg/L, 0.5mg/L, 1.0mg/L:5%HCl medium.
Detecting instrument is existing THERMO iCAP6300 inductively coupled plasma atomic emission spectrometer;
Testing conditions is:
Incident power: 1150W
Atomization gas pressure: 0.18Mpa
Secondary air amount: 0.5L/min
Observed altitude: 8mm
Pump speed: 50rpm
According to the typical curve standard measure.
Result of calculation, the computing formula of inorganic cobalt is in the sample:
The content of inorganic cobalt in the X-sample, unit are every kilogram (mg/kg) of milligram;
C
0-blank solution concentration, unit is every liter (mg/l) of milligram;
C
1-sample solution concentration, unit is every liter (mg/l) of milligram;
V-constant volume, unit are milliliter (ml);
F-sample solution extension rate;
The m-sample quality, unit is gram (g).
Through calculating, the result is:
The content of inorganic cobalt by formula calculates in the sample, and the result is as follows:
Embodiment 2, and the precision of inorganic cobalt content and the recovery detect in the animal feed:
The testing sample of crossing 80 mesh sieves after the drying and crushing takes by weighing 5.1020g, (accurately weighing to 0.0001 gram), place 25ml tool plug scale color comparison tube, add 12% aqueous hydrochloric acid solution to the scale mixing, place 90 ℃ water-bath 4 hours～8 hours, failure of oscillation does not swing therebetween, make the abundant lixiviate of sample, take out cold filtration, blank assay is made in the machine test simultaneously on the filtrate.
Use the Co standard reserving solution: single element solution composition analytical standard material cobalt, 1000mg/L, medium 5%HCl; Preparation Co working solution, concentration gradient 0.0mg/L, 0.1mg/L, 0.5mg/L, 1.0mg/L, 5.0mg/L, 10.0mg/L:5%HC l medium.
Detecting instrument is existing THERMO iCAP6300 inductively coupled plasma atomic emission spectrometer:
Testing conditions:
Incident power: 1150W
Atomization gas pressure: 0.18Mpa
Secondary air amount: 0.5L/min
Observed altitude: 8mm
Pump speed: 50rpm
According to the typical curve standard measure.
Result of calculation, the computing formula of inorganic cobalt is in the sample:
The content of inorganic cobalt in the X-sample, unit are every kilogram (mg/kg) of milligram;
C
0-blank solution concentration, unit is every liter (mg/l) of milligram;
C
1-sample solution concentration, unit is every liter (mg/l) of milligram;
V-constant volume, unit are milliliter (ml);
F-sample solution extension rate;
The m-sample quality, unit is gram (g).
The content of inorganic cobalt by formula calculates in the sample, and the result is as follows:
Obviously, those of ordinary skill in the art, can with of the present invention a kind of by inductively coupled plasma atomic emission spectrometer to inorganic cobalt content detecting method in biochemicals, food, the feed, constitute the method that inorganic cobalt content in all kinds biochemicals, food and the feed is detected.
The foregoing description is only for the usefulness that the present invention is described; and be not to be limitation of the present invention; the those of ordinary skill in relevant technologies field; without departing from the present invention; can also make various variations and modification; therefore all technical schemes that are equal to also should belong to category of the present invention, and scope of patent protection of the present invention should be limited by each claim.
Claims (2)
1. one kind by the assay method of inductively coupled plasma atomic emission spectrometer to inorganic cobalt in biochemicals, food, the feed, and it is characterized in that: described assay method comprises the steps:
1. specimen preparation:
Solid sample is through crossing 80 mesh sieves after the drying and crushing, the bright sample of animal tissue breaks into homogenate;
Take by weighing the sample 5g～10g of animal tissue of the solid sample that sieves or bright sample making beating, place 25ml tool plug scale color comparison tube, add 12% aqueous hydrochloric acid solution to the scale mixing, place 90 ℃ water-bath 4 hours～8 hours, failure of oscillation does not swing therebetween, after making the abundant lixiviate of sample, take out leaching liquor, cooling is with 0.45 μ m membrane filtration, blank assay is made in the machine test simultaneously on the filtrate;
Take by weighing fluid sample 0.5g～10g, place 25ml tool plug scale color comparison tube, add 2% aqueous hydrochloric acid solution to the scale mixing, vibration is 15 minutes under room temperature, leaves standstill the back as if the not muddy supernatant of then getting of leaching liquor, last machine test; If the leaching liquor muddiness places 60 ℃ of water-baths 15 minutes, use 0.45 μ m membrane filtration again, blank assay is made in the machine test simultaneously on the filtrate;
2. go up the machine test: utilize inductively coupled plasma atomic emission spectrometer that standard solution, blank solution and sample treatment solution are detected.
2. a kind of assay method to inorganic cobalt in biochemicals, food, the feed according to claim 1 is characterized in that: the described condition of utilizing inductively coupled plasma atomic emission spectrometer to detect is:
Incident power: 1150W;
Atomization gas pressure: 0.18Mpa;
Secondary air amount: 0.5L/min;
Observed altitude: 8mm;
Pump speed: 50rpm.
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Address after: 266104 Green Chemical Building, No. 36 Jinshui Road, Beizhai Street, Laoshan District, Qingdao City, Shandong Province, 7 floors Patentee after: Qingdao Pony Test Co., Ltd. Address before: 266101 No. 2-1 Keyuan Weisan Road, Laoshan District, Qingdao City, Shandong Province Patentee before: Qingdao Pony Test Co., Ltd. |