CN105588807A - Assay method of sodium and potassium elements in dairy product - Google Patents
Assay method of sodium and potassium elements in dairy product Download PDFInfo
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Abstract
The invention provides an assay method of sodium and potassium elements in dairy products, which includes the steps of 1) weighing 5-15 g of a sample of milk or a dairy product; 2) heating the sample on an electric-heating plate on soft fire until the sample is dry, and carbonizing the sample on micro fire until no smoke is generated; 3) moving the sample in a muffle furnace for ashing the sample until no black particle exists; 4) adding 5 ml of a 20% hydrochloric acid solution to dissolve the ashed sample, moving the solution to a 50 ml volumetric flask, and diluting the solution to scale with water to prepare a sample solution; 5) placing 1 ml of the sample solution in a 50 ml volumetric flask, adding lanthanum and cesium compounds which are acceptable in element assay, diluting the sample solution to scale with 2% hydrochloric acid, and uniformly mixing the solution to prepare a to-be-assayed sample solution, wherein concentration of lanthanum element in the to-be-assayed sample solution is 1-2 mg/ml and mass percentage concentration of cesium element in the to-be-assayed sample solution is 0.0158-0.0316%; and 6) directly detecting the to-be-assayed sample solution with instruments in a manner of an atomic absorption method or an atomic emission method. The method is more excellent in accuracy.
Description
Technical field
The present invention relates to the assay method of constituent content in a kind of food, particularly the assay method of sodium, potassium element in a kind of dairy products.
Background technology
Calcium, potassium, sodium, magnesium, manganese, copper, iron, zinc content detection in infant formula and dairy products, can select the conventional atomic absorption method of element determination and atomic emissions method. Existing " mensuration of calcium, iron, zinc, sodium, potassium, magnesium, copper and manganese in national food safety standard infant food and dairy products " (GB5413.21-2010) has recorded the sample pretreatment process of two kinds of detection methods.
The sample pre-treatments of atomic absorption spectrophotometry is: take the about 5g of the solid sample mixing or the about 15g(of liquor sample is accurate to 0.0001g) in crucible, on electric furnace, low baking temperature charing is to no longer smoldering, move into again in Muffle furnace 490 DEG C ± 5 DEG C about 5h of ashing. If there is black carbon granule, cooling after, drip a little salpeter solution (50%, V/V) moistening. On electric furnace after little fiery evaporate to dryness, then move in 490 DEG C of high temperature furnaces and continue to be ashing into white ashes. After being cooled to room temperature, take out, add 5mL hydrochloric acid (20%, V/V), on electric furnace, heating is fully dissolved ashes. Be cooled to after room temperature, move in 50mL volumetric flask, water constant volume is processed at least two blank samples simultaneously.
The sample pre-treatments of Inductively coupled plasma atomic emission spectrometry method is: take 5g sample (being accurate to 0.001g) in porcelain crucible, on electric furnace, low baking temperature charing is to not smoldering, move into 550 DEG C of heating 2h in Muffle furnace, if any black carbon granule, after cooling, add a little salpeter solution (50%, V/V) moistening, after little fiery evaporate to dryness, move into again in Muffle furnace 550 DEG C of heating half an hour, take out cooling, add hydrochloric acid (40%, V/V) 5mL, on electric furnace, careful heating is fully dissolved ash content, after cooling, be transferred in 25mL volumetric flask, water is settled to scale, if there is precipitation to need to filter. to be measured.
When prior art discloses mensuration calcium, magnesium, need make releasing agent with lanthanum, disturb to eliminate phosphoric acid. But adopt above-mentioned method to detect same sample different time, no matter whether add the compound containing lanthanum, the testing result of sodium, potassium element is had to larger difference. While carrying out parallel test, the testing result of sodium and potassium element also has larger difference. At Wu Chunmin. atomic absorption method and atomic emissions method are measured the comparison of sodium in milk powder, [J] herding and forage science 2009,30(3): 83-84, discloses a kind of cesium chloride using 2g/L as anti-interference agent, the method that sodium element is detected. But this technological means can only be eliminated in the ionization of flame part and disturb, actual in solution potassium, sodium ion ionize (potassium, sodium element ionization potential are lower, easily ionizable in solution, and then the phenomenon such as generation container absorption); Cause after sample liquid has been prepared, the resting period is larger on the impact of testing result and the rate of recovery. If test sample liquid must be now with the current, not only can cause operating efficiency to reduce; Again prepare sample liquid and also can waste reagent, increase the burden of environment. Sodium and potassium have the disturbing factor that is different from calcium, magnesium, therefore need to develop a kind of simple and efficient, detection method that the degree of accuracy is high for sodium, potassium element.
Summary of the invention
The object of this invention is to provide the assay method of sodium, potassium element in a kind of new dairy products, to improve the degree of accuracy of sample detection.
The invention provides the assay method of sodium, potassium element in a kind of dairy products, comprise the following steps: take breast or dairy products sample 5g-15g, on electric hot plate, little fire is heated to do, low baking temperature charing is to no longer smoldering, then moves into and in Muffle furnace, carry out ashing, and ashing is to without black particle, add 5ml20% dissolve with hydrochloric acid solution, move in 50ml volumetric flask, then water is settled to scale, obtains sample dissolution liquid; From sample dissolution liquid, take out 1ml and be placed in 50ml volumetric flask, the compound of acceptable lanthanum element and cesium element in addition element mensuration, be settled to scale with 2% hydrochloric acid again, mix, obtain analyte sample fluid, in analyte sample fluid, lanthanum element concentration is 1-2mg/ml, and in analyte sample fluid, cesium element mass percent concentration is 0.0158-0.0316%; And analyte sample fluid is directly carried out to instrument detection; Instrument detects as atomic absorption method detection or the detection of atomic emissions method.
In dairy products, in a kind of exemplary embodiment of the assay method of sodium, potassium element, in addition element mensuration wherein, the compound step of acceptable lanthanum element and cesium element is: add lanthana and cesium chloride.
In dairy products, in a kind of exemplary embodiment of the assay method of sodium, potassium element, add lanthana and cesium chloride step are wherein: add the lanthana solution 1-2mL of 60g/L and the cesium chloride solution 0.5-1mL that mass percent is 2%.
In dairy products, in a kind of exemplary embodiment of the assay method of sodium, potassium element, instrument wherein detects as atomic absorption method detection.
In dairy products, in a kind of exemplary embodiment of the assay method of sodium, potassium element, instrument wherein detects as atomic emission spectrometry detection.
In dairy products, in a kind of exemplary embodiment of the assay method of sodium, potassium element, atomic emission spectrometry wherein detects as the detection of Inductively coupled plasma atomic emission spectrometry method.
The assay method of sodium, potassium element in dairy products provided by the invention, testing result has better accuracy. The Sample storage time of the present invention is longer, therefore more easily arranges monitoring, has reduced sample and reagent waste, has improved efficiency simultaneously.
Detailed description of the invention
For technical characterictic, object and the effect of invention are had more clearly and understood, the existing the specific embodiment of the present invention that illustrates with the following Examples.
Although adopted lanthana and cesium chloride in embodiment, but be not intended to limit the present invention, the compound of acceptable other lanthanum elements and cesium element in element determination, as lanthanum chloride, lanthanum nitrate, cesium oxide, cesium nitrate etc., also can complete object of the present invention.
Although adopted Inductively coupled plasma atomic emission spectrometry method in embodiment, other atomic emission spectrometries that those skilled in the art are familiar with also can realize object of the present invention.
Embodiment 1.
Take liquid milk sample 5.0105g, on electric hot plate, little fire is heated to do, and low-temperature carbonization is to no longer smoldering, move into again in Muffle furnace and carry out ashing to without black particle, add 5ml20% dissolve with hydrochloric acid solution, move in 50ml volumetric flask, water is settled to scale again, obtains sample dissolution liquid; From sample dissolution liquid, take out 1ml and be placed in 50ml volumetric flask, add the lanthana solution 1mL of 60g/L and the cesium chloride solution 0.5mL that mass percent is 2%, mix with 2% hydrochloric acid constant volume.
Embodiment 2.
Take liquid milk sample 5.0900g, on electric hot plate, little fire is heated to do, and low-temperature carbonization is to no longer smoldering, move into again in Muffle furnace and carry out ashing to without black particle, add 5ml20% dissolve with hydrochloric acid solution, move in 50ml volumetric flask, water is settled to scale again, obtains sample dissolution liquid; From sample dissolution liquid, take out 1ml and be placed in 50ml volumetric flask, add the lanthana solution 2mL of 60g/L and the cesium chloride solution 1mL that mass percent is 2%, mix with 2% hydrochloric acid constant volume.
Embodiment 3.
Take liquid milk sample 5.0082g, on electric hot plate, little fire is heated to do, and low-temperature carbonization is to no longer smoldering, move into again in Muffle furnace and carry out ashing to without black particle, add 5ml20% dissolve with hydrochloric acid solution, move in 50ml volumetric flask, water is settled to scale again, obtains sample dissolution liquid; From sample dissolution liquid, take out 1ml and be placed in 50ml volumetric flask, add the lanthana solution 1.5mL of 60g/L and the cesium chloride solution 0.7mL that mass percent is 2%, mix with 2% hydrochloric acid constant volume.
Embodiment 4.
Take liquid milk sample 9.5762g, on electric hot plate, little fire is heated to do, and low-temperature carbonization is to no longer smoldering, move into again in Muffle furnace and carry out ashing to without black particle, add 5ml20% dissolve with hydrochloric acid solution, move in 50ml volumetric flask, water is settled to scale again, obtains sample dissolution liquid; From sample dissolution liquid, take out 1ml and be placed in 50ml volumetric flask, add the lanthana solution 1.5mL of 60g/L and the cesium chloride solution 0.7mL that mass percent is 2%, mix with 2% hydrochloric acid constant volume.
Embodiment 5.
Take liquid milk sample 15.0215g, on electric hot plate, little fire is heated to do, and low-temperature carbonization is to no longer smoldering, move into again in Muffle furnace and carry out ashing to without black particle, add 5ml20% dissolve with hydrochloric acid solution, move in 50ml volumetric flask, water is settled to scale again, obtains sample dissolution liquid; From sample dissolution liquid, take out 1ml and be placed in 50ml volumetric flask, add the lanthana solution 1mL of 60g/L and the cesium chloride solution 0.5mL that mass percent is 2%, mix with 2% hydrochloric acid constant volume.
Embodiment 6.
Take liquid milk sample 15.0200g, on electric hot plate, little fire is heated to do, and low-temperature carbonization is to no longer smoldering, move into again in Muffle furnace and carry out ashing to without black particle, add 5ml20% dissolve with hydrochloric acid solution, move in 50ml volumetric flask, water is settled to scale again, obtains sample dissolution liquid; From sample dissolution liquid, take out 1ml and be placed in 50ml volumetric flask, add the lanthana solution 2mL of 60g/L and the cesium chloride solution 1mL that mass percent is 2%, mix with 2% hydrochloric acid constant volume.
Embodiment 7.
Take liquid milk sample 14.9962g, on electric hot plate, little fire is heated to do, and low-temperature carbonization is to no longer smoldering, move into again in Muffle furnace and carry out ashing to without black particle, add 5ml20% dissolve with hydrochloric acid solution, move in 50ml volumetric flask, water is settled to scale again, obtains sample dissolution liquid; From sample dissolution liquid, take out 1ml and be placed in 50ml volumetric flask, add the lanthana solution 2mL of 60g/L and the cesium chloride solution 0.5mL that mass percent is 2%, mix with 2% hydrochloric acid constant volume.
Embodiment 8.
Take liquid milk sample 15.0022g, on electric hot plate, little fire is heated to do, and low-temperature carbonization is to no longer smoldering, move into again in Muffle furnace and carry out ashing to without black particle, add 5ml20% dissolve with hydrochloric acid solution, move in 50ml volumetric flask, water is settled to scale again, obtains sample dissolution liquid; From sample dissolution liquid, take out 1ml and be placed in 50ml volumetric flask, add the lanthana solution 1mL of 60g/L and the cesium chloride solution 1mL that mass percent is 2%, mix with 2% hydrochloric acid constant volume.
Embodiment 9:Atomic absorption spectrophotometry.
The sample that embodiment 1 processed detects with atomic absorption spectrophotometer, and detecting instrument condition is: lamp current sodium 5mA, potassium 5mA, and acetylene gas flow 2.4ml/min, slit sodium, potassium are 0.7nm, detection line sodium 589.0nm, potassium 766.4nm.
Embodiment 10:Atomic absorption spectrophotometry.
The sample that embodiment 2 processed detects with atomic absorption spectrophotometer, and detecting instrument condition is: lamp current sodium 5mA, potassium 5mA, and acetylene gas flow 2.4ml/min, slit sodium, potassium are 0.7nm, detection line sodium 589.0nm, potassium 766.4nm.
Embodiment 11:Atomic absorption spectrophotometry.
The sample that embodiment 3 processed detects with atomic absorption spectrophotometer, and detecting instrument condition is: lamp current sodium 5mA, potassium 5mA, and acetylene gas flow 2.4ml/min, slit sodium, potassium are 0.7nm, detection line sodium 589.0nm, potassium 766.4nm.
Embodiment 12:Inductively coupled plasma atomic emission spectrometry method.
The sample that embodiment 1 processed detects with inductively coupled plasma atomic emission, instrument condition: power 1300kw/h, atomizer 0.8L/min, sample size 1.5ml/min.
Embodiment 13:Inductively coupled plasma atomic emission spectrometry method.
The sample that embodiment 2 processed detects with inductively coupled plasma atomic emission, instrument condition: power 1300kw/h, atomizer 0.8L/min, sample size 1.5ml/min.
Embodiment 14:Inductively coupled plasma atomic emission spectrometry method.
The sample that embodiment 3 processed detects with inductively coupled plasma atomic emission, instrument condition: power 1300kw/h, atomizer 0.8L/min, sample size 1.5ml/min.
Embodiment 15:Atomic absorption spectrophotometry.
The sample that embodiment 4 processed detects with atomic absorption spectrophotometer, and detecting instrument condition is: lamp current sodium 5mA, potassium 5mA, and acetylene gas flow 2.4ml/min, slit sodium, potassium are 0.7nm, detection line sodium 589.0nm, potassium 766.4nm.
Embodiment 16:Atomic absorption spectrophotometry.
The sample that embodiment 5 processed detects with atomic absorption spectrophotometer, and detecting instrument condition is: lamp current sodium 5mA, potassium 5mA, and acetylene gas flow 2.4ml/min, slit sodium, potassium are 0.7nm, detection line sodium 589.0nm, potassium 766.4nm.
Embodiment 17:Atomic absorption spectrophotometry.
The sample that embodiment 6 processed detects with atomic absorption spectrophotometer, and detecting instrument condition is: lamp current sodium 5mA, potassium 5mA, and acetylene gas flow 2.4ml/min, slit sodium, potassium are 0.7nm, detection line sodium 589.0nm, potassium 766.4nm.
Embodiment 18:Inductively coupled plasma atomic emission spectrometry method.
The sample that embodiment 7 processed detects with inductively coupled plasma atomic emission, instrument condition: power 1300kw/h, atomizer 0.8L/min, sample size 1.5ml/min.
Embodiment 19:Inductively coupled plasma atomic emission spectrometry method.
The sample that embodiment 8 processed detects with inductively coupled plasma atomic emission, instrument condition: power 1300kw/h, atomizer 0.8L/min, sample size 1.5ml/min.
Comparative example 1:GB5413.21-2010 first method.
The sample pre-treatments of atomic absorption spectrophotometry is: take the about 5.1012g(of the liquor sample mixing and be accurate to 0.0001g) in crucible, on electric furnace, low baking temperature charing is extremely no longer smoldered, then moves in Muffle furnace 490 DEG C ± 5 DEG C about 5h of ashing. If there is black carbon granule, cooling after, drip a little salpeter solution (50%, V/V) moistening. On electric furnace after little fiery evaporate to dryness, then move in 490 DEG C of high temperature furnaces and continue to be ashing into white ashes. After being cooled to room temperature, take out, add 5mL hydrochloric acid (20%, V/V), on electric furnace, heating is fully dissolved ashes. Be cooled to after room temperature, move in 50mL volumetric flask, water constant volume is processed at least two blank samples simultaneously. At sodium 589.0nm, potassium 766.5nm Absorption Line, detect instrument condition: slit 0.5nm, lamp current 5Am, burner height 10 with the Z-2000 of Hitachi type atomic absorption spectrophotometer.
Comparative example 2:GB5413.21-2010 the second method.
The sample pre-treatments of Inductively coupled plasma atomic emission spectrometry method is: take liquor sample 5.0821g sample (being accurate to 0.001g) in porcelain crucible, on electric furnace, low baking temperature charing is to not smoldering, move into 550 DEG C of heating 2h in Muffle furnace, if any black carbon granule, after cooling, add a little salpeter solution (50%, V/V) moistening, after little fiery evaporate to dryness, move into again in Muffle furnace 550 DEG C of heating half an hour, take out cooling, add hydrochloric acid (40%, V/V) 5mL, on electric furnace, careful heating is fully dissolved ash content, after cooling, be transferred in 25mL volumetric flask, water is settled to scale, if there is precipitation to need to filter. to be measured. at sodium 589.0nm, potassium 766.5nm Absorption Line, detect instrument condition: atomizer flow 1.5L/min, power 1300W, throughput 0.85L/min with PEoptima5800 type inductive coupling plasma emission spectrograph.
Comparative example 3.
Take even sample 0.5325g in polytetrafluoroethylene (PTFE) retort, add 10mL red fuming nitric acid (RFNA) sealing, then be put in microwave dissolver (U.S. CE M, microwave dissolver) in, clear up procedure operation according to the intensification of setting, after completing and clearing up, be placed in electric hot plate in fume hood and catch up with acid operation, when acid is caught up with to the greatest extent when remaining 1～2mL liquid in tank, wash in 50mL volumetric flask by deionized water, then add the cesium chloride solution 1mL constant volume of 2g/L to be measured. At sodium 589.0nm, potassium 766.5nm Absorption Line, detect instrument condition: slit 0.5nm, lamp current 5Am, burner height 10 with the Z-2000 of Hitachi type atomic absorption spectrophotometer.
Micro-wave digestion instrument Elevated Temperature Conditions:
| Power | Heating-up time min | Intensification temperature DEG C | Retention time min |
| 1600W | 5 | 120 | 5 |
| 1600W | 2 | 150 | 5 |
| 1600W | 2 | 180 | 20 |
Precision checking.
Precision detects: seven sample detection results of potassium element and sodium element are calculated its precision, with RSD% value representation.
The precision (testing result unit is: mg/100g) that potassium element detects
| Detect number of times | 1 | 2 | 3 | 4 | 5 | 6 | 7 | RSD(%) |
| Embodiment 9 | 132 | 136 | 133 | 139 | 133 | 134 | 135 | 1.76 |
| Embodiment 10 | 135 | 134 | 133 | 135 | 136 | 133 | 133 | 0.91 |
| Embodiment 11 | 145 | 143 | 148 | 146 | 145 | 144 | 145 | 1.08 |
| Embodiment 12 | 144 | 143 | 146 | 146 | 143 | 144 | 146 | 0.97 |
| Embodiment 13 | 140 | 141 | 141 | 140 | 138 | 141 | 140 | 0.76 |
| Embodiment 14 | 141 | 140 | 138 | 139 | 140 | 141 | 139 | 0.8 |
| Embodiment 15 | 142 | 144 | 143 | 144 | 141 | 145 | 142 | 0.99 |
| Embodiment 16 | 146 | 142 | 144 | 141 | 143 | 145 | 142 | 1.26 |
| Embodiment 17 | 144 | 142 | 141 | 145 | 141 | 140 | 145 | 1.45 |
| Embodiment 18 | 144 | 142 | 141 | 140 | 143 | 140 | 145 | 1.37 |
| Embodiment 19 | 142 | 144 | 146 | 140 | 142 | 146 | 143 | 1.55 |
| Comparative example 1 | 132 | 141 | 148 | 135 | 141 | 139 | 150 | 4.59 |
| Comparative example 2 | 133 | 140 | 138 | 150 | 144 | 147 | 148 | 4.28 |
| Comparative example 3 | 132 | 147 | 141 | 139 | 140 | 144 | 150 | 4.14 |
. The embodiment of the present invention is to better (0.76%-1.76%) of the testing result precision of potassium element, and the detection precision of method of comparison is poor comparatively speaking, and RSD all approaches 5%.
The precision (testing result unit is: mg/100g) that sodium element detects
| Detect number of times | 1 | 2 | 3 | 4 | 5 | 6 | 7 | RSD(%) |
| Embodiment 9 | 43.1 | 44 | 42.9 | 44.6 | 42.8 | 43.6 | 43.8 | 1.5 |
| Embodiment 10 | 44.1 | 43.6 | 43.8 | 42.9 | 44.2 | 43.6 | 43.8 | 0.97 |
| Embodiment 11 | 43.6 | 44.1 | 43.9 | 44.5 | 45.2 | 43.6 | 44.1 | 1.27 |
| Embodiment 12 | 44.1 | 43.6 | 44.1 | 45.1 | 44.2 | 43.5 | 44.1 | 1.18 |
| Embodiment 13 | 43.9 | 44.1 | 42.9 | 43.1 | 43.6 | 44.5 | 45 | 1.7 |
| Embodiment 14 | 44.1 | 43.5 | 43.1 | 44.5 | 43.8 | 43.5 | 44.9 | 1.43 |
| Embodiment 15 | 42.6 | 43.5 | 43.9 | 44.1 | 44.8 | 43.8 | 44.1 | 1.53 |
| Embodiment 16 | 43.5 | 43.6 | 44.2 | 42.9 | 44.5 | 43.8 | 43.7 | 1.17 |
| Embodiment 17 | 44.1 | 43.5 | 43.9 | 43.8 | 42.8 | 43.6 | 43.8 | 0.96 |
| Embodiment 18 | 42.4 | 43.5 | 42.9 | 44.6 | 43.8 | 42.9 | 43.6 | 1.67 |
| Embodiment 19 | 44.2 | 44.8 | 43.8 | 42.9 | 43.3 | 43.8 | 44.1 | 1.41 |
| Comparative example 1 | 38.5 | 43.5 | 46.9 | 42.8 | 45.1 | 47 | 43.2 | 6.65 |
| Comparative example 2 | 37.5 | 40.5 | 39.5 | 42.5 | 41.5 | 38.2 | 43.2 | 5.3 |
| Comparative example 3 | 37.1 | 42.5 | 44 | 43.2 | 38.8 | 43.6 | 40.9 | 6.35 |
. The embodiment of the present invention, to better (0.97%-1.7%) of the testing result precision of sodium element, all exceeds 5% and detect precision RSD in method of comparison, still can not meet the needs of analytical work.
Rate of recovery checking.
The rate of recovery: carry out rate of recovery monitoring by the testing result of 10 mark-on samples (adding scalar is: potassium 100mg/100g, sodium 50mg/100g), its result mean value is as following table:
| The potassium element rate of recovery (%) | The sodium element rate of recovery (%) | |
| Embodiment 9 | 100.2 | 99.8 |
| Embodiment 10 | 95.9 | 98.6 |
| Embodiment 11 | 98.2 | 96.5 |
| Embodiment 12 | 99.8 | 100.2 |
| Embodiment 13 | 98.9 | 99.5 |
| Embodiment 14 | 98.9 | 101 |
| Embodiment 15 | 99.6 | 98.5 |
| Embodiment 16 | 98.8 | 100.2 |
| Embodiment 17 | 99.1 | 98.9 |
| Embodiment 18 | 102 | 97.6 |
| Embodiment 19 | 101 | 98.9 |
| Comparative example 1 | 91.5 | 93.8 |
| Comparative example 2 | 93.8 | 95.1 |
| Comparative example 3 | 93.2 | 90.8 |
Better (96.5%-101%) of the rate of recovery of the inventive method can be found out, the needs of analytical work can be met completely; And the rate of recovery of comparative example 1 and comparative example 3 is all lower than 95%. Detection method provided by the invention has significant progress aspect accuracy.
Comparative example 4.
Sample 1: take liquid milk sample 5.1001g, little fire is heated to do on electric hot plate, low-temperature carbonization, move into again in Muffle furnace and carry out ashing to without black particle, add 5ml20% dissolve with hydrochloric acid solution, move in 50ml volumetric flask, water is settled to scale again, obtains sample dissolution liquid; From sample dissolution liquid, take out 1ml and be placed in 50ml volumetric flask, constant volume mixes, and obtains comparative sample 1 standing time.
Sample 2: take fluid milk breast sample 5.0579g, little fire is heated to do on electric hot plate, low-temperature carbonization, move into again in Muffle furnace and carry out ashing to without black particle, add 5ml20% dissolve with hydrochloric acid solution, move in 50ml volumetric flask, water is settled to scale again, obtains sample dissolution liquid; From sample dissolution liquid, take out 1ml and be placed in 50ml volumetric flask, adding mass percent is 2% cesium chloride solution 0.5mL, and constant volume mixes, and obtains comparative sample 2 standing time.
Sample 3: take same liquid breast sample 5.1005g, carry out pre-treatment according to the method for embodiment 1, obtain comparative sample 3 standing time.
After above-mentioned sample solution preparation, detect immediately; And at ambient temperature, place 1 hour, place and within 3 hours, detect respectively (detection method is identical with embodiment 4), testing result is shown in following table:
Different time sections detects sodium, potassium content testing result
| Detect immediately | Place 1 hour | Place 3 hours | |
| Standing time comparative sample 1(potassium element, the mg/100g of unit) | 145 | 130 | 128 |
| Standing time comparative sample 1(sodium element, the mg/100g of unit) | 41.5 | 35.2 | 35.2 |
| Standing time comparative sample 2(potassium element, the mg/100g of unit) | 143 | 132 | 125 |
| Standing time comparative sample 2(sodium element, the mg/100g of unit) | 41.9 | 33.6 | 31.7 |
| Standing time comparative sample 3(potassium element, the mg/100g of unit) | 141 | 129 | 133 |
| Standing time comparative sample 3(sodium element, the mg/100g of unit) | 42 | 41.8 | 41.5 |
Different time sections detects sodium, potassium content detects the rate of recovery, method of operating is as follows: to adding respectively 40mg/100g, 50mg/100g sodium element standard items in the sample taking, 100mg/100g, 120mg/100g potassium element standard items, still according to comparative sample 1-3 method preparation standing time described in comparative example 4; After above-mentioned sample solution preparation, detect immediately; And at ambient temperature, place 1 hour, place and within 3 hours, detect respectively (detection method is identical with comparative example 1). The mean value of the different time sections rate of recovery is as follows.
Different time sections detects sodium, potassium content detects rate of recovery result
| Detect immediately | Place 1 hour | Place 3 hours | |
| Standing time comparative sample 1(potassium element, %) | 92.3 | 85.6 | 81.6 |
| Standing time comparative sample 1(sodium element, %) | 90.1 | 88.1 | 89.1 |
| Standing time comparative sample 2(potassium element, %) | 89.2 | 85.6 | 80.6 |
| Standing time comparative sample 2(sodium element, %) | 88.3 | 82.5 | 83.0 |
| Standing time comparative sample 3(potassium element, %) | 95.9 | 99.6 | 101 |
| Standing time comparative sample 3(sodium element, %) | 98.6 | 98.5 | 98.7 |
From above data, technical scheme of the present invention has not only been improved precision and the rate of recovery of existing detection method, further can also effectively extend the standing time of test sample liquid, at least can extend to 3 hours. Not only reduce the waste of reagent and sample, significantly improved operating efficiency simultaneously.
In this article, " schematically " expression " is served as example, example or explanation ", any embodiment that is described in this article " schematically " should be interpreted as a kind of preferred or have more the technical scheme of advantage.
In this article, " equating ", " identical " etc. are not the restriction in strict mathematics and/or geometry meaning, also comprise the error it will be appreciated by those skilled in the art that and production or use etc. allow. Except as otherwise noted, number range herein not only comprises the gamut in two end points, also comprises the some subranges that are contained in wherein.
Be to be understood that, although this description is described according to each embodiment, but be not that each embodiment only comprises an independently technical scheme, this narrating mode of description is only for clarity sake, those skilled in the art should make description as a whole, technical scheme in each embodiment also can, through appropriately combined, form other embodiments that it will be appreciated by those skilled in the art that.
Listed a series of detailed description is above only illustrating for feasibility embodiment of the present invention; they are not in order to limit the scope of the invention; allly do not depart from equivalent embodiment or the change that skill spirit of the present invention is done; as the combination of feature, cut apart or repeat, within all should being included in protection scope of the present invention.
Claims (6)
1. an assay method for sodium, potassium element in dairy products, is characterized in that, comprises the following steps:
Take breast or dairy products sample 5g-15g, on electric hot plate, little fire is heated to do, low baking temperature charing is to no longer smoldering, move into again and in Muffle furnace, carry out ashing, ashing, to without black particle, adds 5ml20% dissolve with hydrochloric acid solution, moves in 50ml volumetric flask, water is settled to scale again, obtains sample dissolution liquid;
From described sample dissolution liquid, take out 1ml and be placed in 50ml volumetric flask, the compound of acceptable lanthanum element and cesium element in addition element mensuration, be settled to scale with 2% hydrochloric acid again, mix, obtain analyte sample fluid, in described analyte sample fluid, lanthanum element concentration is 1-2mg/ml, and in described analyte sample fluid, cesium element mass percent concentration is 0.0158%-0.0316%; And
Described analyte sample fluid is directly carried out to instrument detection; Described instrument detects as atomic absorption method detection or the detection of atomic emissions method.
2. the assay method of sodium, potassium element in dairy products according to claim 1, in wherein said addition element mensuration, the compound step of acceptable lanthanum element and cesium element is: add lanthana and cesium chloride.
3. the assay method of sodium, potassium element in dairy products according to claim 2, wherein said add lanthana and cesium chloride step are: add the lanthana solution 1-2mL of 60g/L and the cesium chloride solution 0.5-1mL that mass percent is 2%.
4. the assay method of sodium, potassium element in dairy products according to claim 1, wherein said instrument detects as atomic absorption method detection.
5. the assay method of sodium, potassium element in dairy products according to claim 1, wherein said instrument detects as atomic emission spectrometry detection.
6. the assay method of sodium, potassium element in dairy products according to claim 5, wherein said atomic emission spectrometry detects as the detection of Inductively coupled plasma atomic emission spectrometry method.
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