CN1837824A - Ultraviolet auxiliary extraction and hydride generation-atomic fluorescence spectrometry method for determining lead content in blood and extractor therefor - Google Patents
Ultraviolet auxiliary extraction and hydride generation-atomic fluorescence spectrometry method for determining lead content in blood and extractor therefor Download PDFInfo
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Abstract
This invention relates to an ultraviolet auxiliary extraction and hydride generation-atomic fluorescence spectrometry method for determining lead content in blood and extractor therefor. First, for blood pre-process, loading carrying-current to vibrate and mix with blood sample, taking centrifugation, and putting the tube into UV-assist extractor for processing; second, measuring the standard curve for obtained lead with hydride AES; third, forcing the carrying-current with sample liquid to react with the reducer on reaction block and generate plumbane; using the carrying-gas to send the plumbane to atomizer, and detecting the spectrum signal with atomic spectroscopy to compare with the standard curve. Besides, the extractor comprises a non-transparent shell, one or more UV lamps in the shell, and a sample container on side or around the lamp. This invention is more reliable and accurate, and special fit to spread in establishment medical unit.
Description
Technical field
The present invention relates to a kind of ultraviolet assisted extraction and handle blood sample, measure the method and the ultraviolet assisted extraction instrument of lead content in the blood sample then with hydride generation-atomic spectroscopy.
Background technology
Lead is a kind of famous poisonous element, can cause alimentary canal, and hemopoietic system and nervous system are impaired, and is very big to human body (particularly children) harm.But lead is widely used in fields such as accumulator, gasoline knock-reducer, alloy, radioactivity protection again simultaneously, can't thoroughly eliminate in a short time.This has just caused comparatively serious saturnism, particularly is in the children of growth and development stage, and saturnine ratio is very high, probably endangers the whole population quality of China.Saturnine control comprises primary prevention (stopping using doped fuel, apparatus and paint etc.) and secondary prevention (carrying out the children ' s lead poisoning examination in maternal and child care project and other public health projects) and takes non-pharmaceutical method to treat means prevention children ' s lead poisonings such as saturnism.Carry out secondary prevention, just need the lead content in the human body, for government formulates the relevant laws rules, the control saturnism provides scientific basis.On the other hand, patient is carried out clinical lead content detect, will help to judge the cause of disease, provide strong foundation for formulating correct therapeutic scheme.
Current detection human body lead content mainly relies on the detection to blood lead, and main method has zinc protoporphyrin method, differetial-potential leaching, graphite oven atomic absorption, hydride generation-atomic spectroscopy etc.Wherein preceding two kinds of method detection limits are higher, and accuracy of measurement is relatively poor, seldom use now; Graphite oven atomic absorption is the standard method that current blood lead is measured, but its instrument cost is higher, and operation is comparatively complicated, is difficult to be generalized to grass-roots unit in the such developing country of China.Hydride generation-atomic spectroscopy is used for blood lead and measures practice has preferably been arranged in recent years, this method can really accomplish trace, accurately, cheap, measure blood lead easily, so be highly susceptible to promoting.
Current, adopt hydride generation-atomic spectroscopy to survey blood lead and still have some defectives, mainly concentrate on two aspects: require sample is cleared up when at first being hydride generation-atomic spectroscopy survey blood lead, digestion process length consuming time and easily pollution, acid also can't be caught up with totally; On the other hand, the acidity to reaction when hydride takes place to survey blood lead requires very harshness, and available acidity scope has deviation will cause measurement result significantly on the low side less than 0.5% (percent by volume) slightly; The 3rd, in blood, tend to exist some organic complexing agents, these organic complexing agents can disturb plumbous hydride generating process, make measurement result significantly on the low side.
Summary of the invention
The purpose of this invention is to provide a kind of ultraviolet assisted extraction hydride generation-atomic spectroscopy and measure the method and the extraction apparatus of blood lead.
The purpose of the method for the invention is to be achieved through the following technical solutions:
A kind of method with hydride generation-atomic spectroscopy measurement blood lead content, step are divided into the pre-treatment of first step blood sample, the foundation and the 3rd step sample determination of the second step typical curve.The pre-treatment of described first step blood sample is every current-carrying that adds 2.9 milliliters～2.95 milliliters in the centrifuge tube after the cleaning, add 50～100 microlitre blood samples then and vibrate and mix, left standstill 2～10 minutes, under 3000～12000 rev/mins of rotating speeds centrifugal 2～15 minutes then, again centrifuge tube is put into ultraviolet assisted extraction instrument and handled 5～20 minutes, obtain the sample liquid to be measured of clear; The foundation of the second step typical curve, with the plumbous standard solution stepwise dilution of the 1000 mg/litre standard solution that is the variable concentrations of 0～10 micrograms per litre, measure the typical curve that obtains lead with hydride generation-atomic spectroscopy, this process comprises that current-carrying carries standard solution and reacts with reductive agent to the reaction block place, generate the hydride of the lead of gaseous state, the alanate of gaseous state is delivered to atomization in the atomizer by carrier gas then, record corresponding spectral signal with atomic spectroscopy, just can obtain plumbous typical curve with concentration of standard solution and spectral signal mapping; The 3rd step sample determination, use hydride generation method-atomic spectroscopy working sample liquid to be measured, this process comprises that current-carrying carries sample liquid to be measured and reacts with reductive agent to the reaction block place, generate the hydride of the lead of gaseous state, the alanate of gaseous state is delivered to atomization in the atomizer by carrier gas then, record corresponding spectral signal with atomic spectroscopy, more quantitative with typical curve.
Wherein, the component of described reductive agent is potassium borohydride or sodium borohydride, the potassium ferricyanide of 10 grams per liters-30 grams per liter and the weak acid of 5 grams per liters-20 grams per liter of the NaOH of 10 grams per liters-30 grams per liter or potassium hydroxide, 5 grams per liters-30 grams per liter;
Described weak acid is tartrate, oxalic acid or boric acid.
Described current-carrying is a kind of mixed solution, wherein contains percent by volume and be the mixed solution of the oxidizing agent solution of 1.0%～4.5% inorganic acid and volume or mass percent 1.0～5.0%.
Described inorganic acid is hydrochloric acid, nitric acid, perchloric acid or sulfuric acid.
Described oxidizing agent solution is hydrogen peroxide, potassium persulfate.
Hydride-generation atomic fluorescence of the present invention is surveyed the ultraviolet assisted extraction instrument of blood lead, it is characterized in that: comprise lighttight housing, be provided with an above uviol lamp in housing, the one side of lamp or be provided with the container of depositing sample all around.
Described container is the sample hose that is placed on the support.
Described container is the processing pipeline that is coiled on the uviol lamp.
The two ends of described processing pipeline are provided with stop valve.
The present invention has used a kind of new simple and convenient blood lead disposal route, and by experiment repeatedly, obtain a kind of novel reagent proportioning, enlarged the available acidity scope of measuring, make that the data of measuring are more reliable and more stable, the consumptive material of experiment also is dirt cheap, and method is accurate, quick, convenient, is very suitable for promoting at different medical unit.
The sampling Graphite Furnace Atomic Absorption method of the present invention and standard is relatively, and is simple to operate, fast and also accuracy high, the repeatability of determination data and collimation are good; Main is the low price of instrument, and method of operating simply is convenient to grasp, and the consumptive material of experiment is common chemical reagent, and is with low cost, is very suitable for promoting in the medical institutions of basic unit.
This method is compared with traditional hydride generation-atomic spectrum method, has the following advantages:
1. blood sample pre-treating method of the present invention has avoided traditional hydride generation-atomic spectrum sounding lead method to carry out long-time complicated digestion process to blood sample, has reduced contamination of heavy, and has avoided catching up with sour incomplete problem.
2. the pre-treating method of employing ultraviolet assisted extraction blood lead of the present invention can make the organic complexing agent in the blood sample clear up fully, has avoided the interference of organic complexing agent to the hydride generating process of lead, has avoided measurement result significantly on the low side.
3. improved the reagent that hydride reacts, made available acidity range expansion that hydride reacts, guaranteed the stability and the reliability of measuring process to percent by volume 1.5%.
4. method of the present invention can add current-carrying adds a cover preservation in the centrifuge tube, be easy to carry and preserve, and can very easily blood sample be adopted in the centrifuge tube that adds current-carrying when taking blood sample, adds a cover and avoids contaminated.Use hydro-extractor capacious, once can more than 100 sample of centrifugal treating, can greatly improve the speed of measurement.
5. the experiment consumptive material that method of the present invention is used all is very common, cheap, greatly reduces financial cost.
Description of drawings
Fig. 1 is the structural representation of an embodiment of ultraviolet assisted extraction instrument of the present invention, and expression is static extracts;
Fig. 2 is the structural representation of another embodiment of ultraviolet assisted extraction instrument of the present invention, the expression Dynamic Extraction.
Embodiment
The method that ultraviolet assisted extraction hydride generation-atomic spectroscopy of the present invention is measured blood lead content comprises: the pre-treatment of first step blood sample, the foundation of the second step typical curve, the 3rd step sample determination.
The pre-treatment of first step blood sample, it is every current-carrying that adds 2.9 milliliters～2.95 milliliters in the centrifuge tube after the cleaning, add 50～100 microlitre blood samples then and vibrate and mix, left standstill again 2～10 minutes, under 3000～12000 rev/mins of rotating speeds centrifugal 2～15 minutes then, again centrifuge tube is put into ultraviolet assisted extraction instrument and handled 5～20 minutes, obtain the sample liquid to be measured of clear; The foundation of the second step typical curve, a plurality of standard solution with the plumbous standard solution stepwise dilution of the 1000 mg/litre variable concentrations that is 0～10 micrograms per litre, general desirable 3-6 point, measure the typical curve that obtains lead with hydride generation-atomic spectroscopy, this process comprises that current-carrying carries standard solution and follows to the reaction block place
Reductive agentReaction, the hydride of the lead of generation gaseous state, the alanate of gaseous state is delivered to atomization in the atomizer by carrier gas then, records corresponding spectral signal with atomic spectroscopy, just can obtain plumbous typical curve with concentration of standard solution and spectral signal mapping; The 3rd step sample determination uses hydride generation method-atomic spectroscopy working sample liquid to be measured, and this process comprises that current-carrying carries sample liquid to be measured and follows to the reaction block place
Reductive agentReaction, the hydride of the lead of generation gaseous state, the alanate of gaseous state is delivered to atomization in the atomizer by carrier gas then, records corresponding spectral signal with atomic spectroscopy, and is more quantitative with typical curve.
Described vibration can be adopted equipment such as vortex mixer or ultrasonic mixer, and the about 10-60 of duration of oscillation gets final product second.
The method of mensuration blood lead content of the present invention is on prior art scheme basis, study the influence of factors such as acidity, carrier gas flux, shield gas flow amount, reductive agent proportioning, hollow cathode lamp current, thereby obtained the condition that hydride generation method is measured blood lead; And investigated the influence of interfering ion, common bivalent cation in the whole blood: magnesium (Mg
2+), iron (Fe
3+), zinc (Zn
2+), cobalt (Co
2+), cadmium (Cd
2+), nickel (Ni
2+), calcium (Ca
2+), copper (Cu
2+) waiting 8 kinds of ions, their physiological concentration does not have significantly interference to atom fluorimetry is plumbous, so this method has selectivity preferably.This method has been improved original hydride generation reagent, wherein key component of the reductive agent that uses of second and third step has: the potassium ferricyanide of the potassium borohydride of the NaOH of 10 grams per liters-30 grams per liter or potassium hydroxide, 5 grams per liters-30 grams per liter or sodium borohydride, 10 grams per liters-30 grams per liter and add 5 grams per liters-20 grams per liter weak acid.
Described weak acid can be tartrate, oxalic acid or boric acid etc.
Described current-carrying is a kind of mixed solution, wherein contains percent by volume and be the mixed solution of the oxidizing agent solution of 1.0%～4.5% inorganic acid and volume or mass percent 1.0～5.0%.
Described inorganic acid is hydrochloric acid, nitric acid, perchloric acid or sulfuric acid.
Described oxygenant is hydrogen peroxide, potassium persulfate etc.
Extraction apparatus of the present invention is the instrument that first step medium ultraviolet assisted extraction is handled.Referring to Fig. 1 and Fig. 2, hydride-generation atomic fluorescence of the present invention is surveyed the ultraviolet assisted extraction instrument of blood lead, comprises lighttight housing, is provided with an above uviol lamp 1 in housing, the one side of lamp or be provided with the container of depositing sample all around.
Described container can be the sample hose 2 that is placed on the support.When uviol lamp is many, can be set to two rows by uviol lamp, sample hose 2 is arranged between two bank lights.
Described container can also be the processing pipeline 3 that is coiled on the uviol lamp.Establish at the two ends of processing pipeline and stop valve 4 can be set or stop valve is not set.
Shown in Figure 1 is the static instrument that extracts, and so-called static extraction instrument is that blood sample remains static in processing procedure.During use, will the container 2 (employing centrifuge tube) of sample be housed, insert support, closure casing leaks with preventing ultraviolet, lights and extinguishes uviol lamp after uviol lamp is handled, and takes out sample hose and gets final product.
Shown in Fig. 2 is the Dynamic Extraction instrument, and promptly blood sample is in flow state in the Dynamic Extraction instrument.Its operating process is for to squeeze into processing pipeline with sample by external infusion set, and the stop valve 4 at pipeline two ends can be closed (half dynamically), also can not close (dynamically complete), according to the length of state respective design uviol lamp quantity and pipeline; Closure casing leaks with preventing ultraviolet, after lighting uviol lamp and handling, extinguishes uviol lamp, and the liquid in the processing pipeline is returned centrifuge tube by infusion set.The full dynamical fashion of Dynamic Extraction instrument wherein can directly apply on sequential injection-hydride generation-atomic fluorescence device, the sampling ring that replaces this instrument (is seen CN01274858.7, name is called " the sequential injection sampling device that is used for atomic fluorescence spectrometer "), effect is identical.
Venous blood or tip blood or employing heparin or the ethylenediamine tetraacetic acid of the actual blood sample that uses among the present invention for extracting
(EDTA) venous blood of anti-freezing, wherein the venous blood of anti-freezing can directly be measured or be placed in the refrigerator and preserve a period of time (must not above 3 months) back and measures.
Be the accuracy of the method for inspection, the accepted standard material is from the freeze-drying ox blood GBW09139 and the GBW09140 of CDC, and their calibration value is respectively 96 ± 20ppb and 248 ± 35ppb.
The pre-treatment of first step blood sample, every current-carrying that adds 2.9 milliliters in the centrifuge tube after the cleaning contains percent by volume and is 3.5% the nitric acid and the H of percent by volume 1.0% in the current-carrying
2O
2Add the blood sample that 100 microlitres contain organic complexing agent iminodiacetic acid (IDA) then, be equivalent to dilute 30 times, get 4 centrifuge tubes after the cleaning in addition, every adds 3 milliliters percent by volume is 3.5% nitric acid, as reagent blank, with above-mentioned all centrifuge tubes all on vortex mixer vibration mixed 30 seconds, left standstill again 10 minutes, descended centrifugal 10 minutes at 3000 rev/mins then, centrifugal finishing puts into centrifuge tube static ultraviolet assisted extraction instrument to handle 5～20 minutes again, obtain the sample liquid to be measured of clear, be placed on the specimen holder centrifuge tube taking-up to be measured;
The foundation of the second step typical curve, the plumbous standard solution (GBW08611) that with percent by volume is 3.5% nitric acid stepwise dilution 1000 mg/litre is to 10 micrograms per litre, get five points of 0,2,4,8,10 micrograms per litre then, with 30 grams per liter NaOH+10 grams per liter potassium borohydrides+20 grams per liter potassium ferricyanides+10 grams per liter boric acid is reductive agent, and percent by volume is 3.5% nitric acid
(HNO
3) be current-carrying, (see patent No. CN01274858.7 with sequential injection hydride generation-atomic fluorescence spectrometer, denomination of invention " the sequential injection sampling device that is used for atomic fluorescence spectrometer ") measures the typical curve that can obtain lead, the condition enactment of instrument sees Table 1, and the condition enactment of sequential injection sees Table 2.
The 3rd step sample determination adopts sequential injection hydride generation-atomic fluorescence spectrometer, uses and identical conditioned measurement sample liquid to be measured of second step, obtains the lead content in the blood sample.
Introduce the experimental data of one group of sample below, in experiment, adopt respectively and use the ultraviolet assisted extraction and do not use ultraviolet assisted extraction hydride Generation-Atomic Fluorescence Spectrometry to measure 2 parts of standard lyophilization ox blood sample and 14 parts of venous samples can that contain the anticoagulant heparin of organic complexing agent iminodiacetic acid (IDA) that contain organic complexing agent iminodiacetic acid (IDA), every part of 2 in blood sample work is parallel.Measured 14 parts of venous samples can that contain the anticoagulant heparin of organic complexing agent iminodiacetic acid (IDA) with graphite oven atomic absorption simultaneously, the measurement result that obtains is shown in table 3.
As shown in Table 3, two groups of blood lead values of the GBW09139 that this method records, GBW09140 all drop in the range of uncertainty of mark thing, this method are described accurately and reliably; And the result who does not use the ultraviolet assisted extraction to obtain is significantly on the low side, should be the Gu of organic complexing agent iminodiacetic acid (IDA) interference measurement.In addition, as shown in Table 4, sampling Graphite Furnace Atomic Absorption is passed through paired t-test with the blood lead measurement result of ultraviolet assisted extraction-hydride generation-atomic fluorescence, two kinds of methods of hydride generation-atomic fluorescence respectively, obtain ultraviolet assisted extraction-hydride generation-atomic fluorescence method and sampling Graphite Furnace Atomic Absorption t=-1.59, P=0.135＞0.05, in 95% fiducial interval range, therefore these two kinds of methods are measured blood lead content does not have significant difference, and this has also proved the reliability of method provided by the invention; And do not use the hydride generation-atomic fluorescence method and the sampling Graphite Furnace Atomic Absorption t=8.94 of ultraviolet assisted extraction, and P=0＜0.05, there were significant differences, should be the Gu of organic complexing agent iminodiacetic acid (IDA) interference measurement.Above presentation of results ultraviolet assisted extraction-hydride generation-atomic fluorescence method can well be eliminated organic complexing agent is measured blood lead to hydride generation-atomic fluorescence method interference.
Table 1. hydride generation-atomic fluorescence sounding lead instrument condition
| Total current (mA) | 40～80 | Carrier gas (mL/min) | 300～800 |
| Auxilliary cathode current (mA) | 15～40 | Shielding gas (mL/min) | 600～1000 |
| Negative high voltage (V) | 250～300 | Integral time (s) | 5～12 |
| Body of heater height (mm) | 8～12 | Sampling delay (s) | 1～3 |
| Sample size (mL) | 0.8 | Reading mode | Peak area |
The sequential injection condition of table 2. hydride generation-atomic fluorescence sounding lead
| Time (s) | The sample syringe pump | The multidigit valve position | The reductive agent syringe pump | The wriggling pump speed | Reading | Automatically preparation | |||||
| Valve position | Action | Volume | Valve position | Action | Volume | Sample | Blank | ||||
| 1 | A | Inhale | 1.5 | G | B | Inhale | 0 | 130 | |||
| 1 | B | Inhale | 0.8 | G | B | Inhale | 0 | 0 | |||
| 1 | B | Push away | 2.3 | E | B | Push away | 0 | 0 | |||
| 0.5 | A | Inhale | 1.6 | G | B | Inhale | 1.85 | 130 | √ | ||
| 0.5 | B | Inhale | 0.8 | G | B | Inhale | 1 | 0 | √ | ||
| 0.5 | B | Inhale | 1.2 | G | B | Push away | 0.5 | 0 | |||
| 6 | B | Push away | 3.6 | B | A | Push away | 2.35 | 140 | √ | ||
Table 3. sampling Graphite Furnace Atomic Absorption and the contrast of hydride generation-atomic fluorescence blood lead experimental result
| Sample number | Sampling Graphite Furnace Atomic Absorption (micrograms per litre) | Ultraviolet assisted extraction atomic fluorescence (micrograms per litre) | Atomic fluorescence (micrograms per litre) |
| GBW09139 (96 ± 20 micrograms per litre) | 91±7(S.D.) | 24±15(S.D.) |
| GBW09140 (248 ± 35 micrograms per litre) | 253±6(S.D.) | 67±37(S.D.) | |
| |
62 | 60 | 15 |
| |
42 | 36 | 0 |
| |
53 | 57 | 32 |
| Blood sample 4 | 51 | 53 | 11 |
| Blood sample 5 | 88 | 92 | 31 |
| Blood sample 6 | 102 | 106 | 24 |
| Blood sample 7 | 55 | 56 | 0 |
| Blood sample 8 | 67 | 80 | 12 |
| Blood sample 9 | 50 | 63 | 21 |
| Blood sample 10 | 82 | 90 | 0 |
| Blood sample 11 | 134 | 119 | 45 |
| Blood sample 12 | 145 | 158 | 44 |
| Blood sample 13 | 48 | 54 | 0 |
| Blood sample 14 | 51 | 52 | 12 |
Table 4. paired t-test result
| Pairing | Mean value | Standard deviation | Standard error mean value | 95% fiducial interval | The t value | P |
| Sampling Graphite Furnace Atomic Absorption-ultraviolet assisted extraction-hydride generation-atomic fluorescence | -3.29 | 7.72 | 2.06 | -7.74＜t＜1.17 | -1.59 | 0.135 |
| Sampling Graphite Furnace Atomic Absorption-hydride generation-atomic fluorescence | 55.93 | 23.40 | 6.25 | 42.42＜t＜69.44 | 8.94 | 0.000 |
Embodiment 2:
The pre-treatment of first step blood sample, in the centrifuge tube after the cleaning every to add 2.95 milliliters percent by volume be that 4.5% hydrochloric acid is current-carrying, add the blood sample that 50 microlitres contain organic complexing agent triacetic acid base ammonia (NTA) then, be equivalent to dilute 60 times, get 4 centrifuge tubes after the cleaning in addition, every adds 3 milliliters percent by volume is 4.5% hydrochloric acid, as reagent blank, with above-mentioned all centrifuge tubes all on ultrasonator vibration mixed 60 seconds, left standstill again 2 minutes, descended centrifugal 5 minutes at 10000 rev/mins then, centrifugal finishing, again centrifuge tube is put into dynamic ultraviolet assisted extraction instrument and handled 5～20 minutes, obtain the sample liquid to be measured of clear, be placed on the specimen holder centrifuge tube taking-up to be measured;
The foundation of the second step typical curve, the plumbous standard solution (GBW08611) that with percent by volume is 4.5% hydrochloric acid stepwise dilution 1000 mg/litre is to 10 micrograms per litre, get five points of 0,2,4,8,10 micrograms per litre then, with 30 grams per liter potassium hydroxide+30 grams per liter sodium borohydrides+30 grams per liter potassium ferricyanides+5 grams per liter oxalic acid is reductive agent, percent by volume is that 4.5% hydrochloric acid is current-carrying, can obtain plumbous typical curve with hydride generation-atomic absorption spectrometry, the condition enactment of instrument sees Table 5.
The 3rd step sample determination adopts hydride generation-Atomic Absorption Spectrometer, uses and identical conditioned measurement sample liquid to be measured of second step, obtains the lead content in the blood sample.
Two groups of blood lead values of the GBW09139 that the present embodiment method records, GBW09140 are respectively 97 and 236, all drop in the range of uncertainty of mark thing, this method are described accurately and reliably.
Table 5. hydride generation-atomic absorption instrument condition
| Wavelength | 283.3nm | Spectrum can be with | 0.4nm |
| Lamp current | 3.0mA | Flow rate of carrier gas | 160ml/min |
| The quartz ampoule heating voltage | 150V |
The pre-treatment of first step blood sample, in the centrifuge tube after the cleaning every to add 2.95 milliliters percent by volume be that 2% perchloric acid is current-carrying, add the blood sample that 50 microlitres contain organic complexing agent triacetic acid base ammonia (NTA) then, be equivalent to dilute 60 times, get 4 centrifuge tubes after the cleaning in addition, every adds 3 milliliters percent by volume is 2% perchloric acid, as reagent blank, with above-mentioned all centrifuge tubes all on ultrasonator vibration mixed 50 seconds, left standstill again 4 minutes, descended centrifugal 7 minutes at 8000 rev/mins then, centrifugal finishing, again centrifuge tube is put into dynamic ultraviolet assisted extraction instrument and handled 5～20 minutes, obtain the sample liquid to be measured of clear, be placed on the specimen holder centrifuge tube taking-up to be measured;
The foundation of the second step typical curve, the plumbous standard solution (GBW08611) that with percent by volume is 2% perchloric acid stepwise dilution 1000 mg/litre is to 10 micrograms per litre, get five points of 0,2,4,8,10 micrograms per litre then, with 15 grams per liter potassium hydroxide+5 grams per liter sodium borohydrides+10 grams per liter potassium ferricyanides+20 grams per liter tartrate is reductive agent, percent by volume is that 2% perchloric acid is current-carrying, measure the typical curve that can obtain lead with hydride generation-atomic fluorescence spectrometer, the condition enactment of instrument sees Table 6.
The 3rd step sample determination adopts hydride generation-atomic fluorescence spectrometer, uses and identical conditioned measurement sample liquid to be measured of second step, obtains the lead content in the blood sample.
Two groups of blood lead values of the GBW09139 that the present embodiment method records, GBW09140 are respectively 91 and 253, all drop in the range of uncertainty of mark thing, this method are described accurately and reliably.
Table 6. hydride generation-atomic fluorescence sounding lead instrument condition
| Total current (mA) | 40～80 | Carrier gas (mL/min) | 300～800 |
| Auxilliary cathode current (mA) | 15～40 | Shielding gas (mL/min) | 600～1000 |
| Negative high voltage (V) | 250～300 | Integral time (s) | 5～12 |
| Body of heater height (mm) | 8～12 | Sampling delay (s) | 1～3 |
| Sample size (mL) | 1.2 | Reading mode | Peak area |
Embodiment 4
The pre-treatment of first step blood sample, in the centrifuge tube after the cleaning every to add 2.95 milliliters percent by volume be that 1% sulfuric acid is current-carrying, add the blood sample that 50 microlitres contain organic complexing agent iminodiacetic acid (IDA) then, be equivalent to dilute 60 times, get 4 centrifuge tubes after the cleaning in addition, every adds 3 milliliters percent by volume is 1% sulfuric acid, as reagent blank, with above-mentioned all centrifuge tubes all on vortex mixer vibration mixed 50 seconds, left standstill again 4 minutes, descended centrifugal 2 minutes at 12000 rev/mins then, centrifugal finishing, again centrifuge tube is put into static ultraviolet assisted extraction instrument and handled 5～20 minutes, obtain the sample liquid to be measured of clear, be placed on the specimen holder centrifuge tube taking-up to be measured;
The foundation of the second step typical curve, the plumbous standard solution (GBW08611) that with percent by volume is 1% sulfuric acid stepwise dilution 1000 mg/litre is to 10 micrograms per litre, get five points of 0,2,4,8,10 micrograms per litre then, with 10 grams per liter potassium hydroxide+20 grams per liter sodium borohydrides+15 grams per liter potassium ferricyanides+5 grams per liter citric acids is reductive agent, percent by volume is that 1% sulfuric acid is current-carrying, measure the typical curve that can obtain lead with hydride generation-inductive coupling plasma emission spectrograph, the condition enactment of instrument sees Table 7.
The 3rd step sample determination adopts hydride generation-inductive coupling plasma emission spectrograph, uses and identical conditioned measurement sample liquid to be measured of second step, obtains the lead content in the blood sample.
The blood lead value that the GBW09139 that the present embodiment method records, GBW09140 are two groups is respectively 90 and 251, all drops in the range of uncertainty of mark thing, this method is described accurately and reliably.
Table 7. hydride generation-inductive coupling plasma emission spectrograph condition
| Power | 1.2kW | Wavelength | 220.353nm |
| Height of observation | 11mm | Nebulizer gas pressure | 360kPa |
| The cold gas flow velocity | 14L/min |
Claims (10)
1. ultraviolet assisted extraction hydride generation-atomic spectroscopy is measured the method for blood lead, step is divided into the pre-treatment of first step blood sample, the foundation of the second step typical curve and the 3rd step sample determination, it is characterized in that: the pre-treatment of described first step blood sample is every current-carrying that adds 2.9 milliliters～2.95 milliliters in the centrifuge tube after the cleaning, add 50～100 microlitre blood samples then and vibrate and mix, left standstill again 2～10 minutes, under 3000～12000 rev/mins of rotating speeds centrifugal 2～15 minutes then, again centrifuge tube is put into ultraviolet assisted extraction instrument and handled 5～20 minutes, obtain the sample liquid to be measured of clear; The foundation of the second step typical curve, with the plumbous standard solution stepwise dilution of the 1000 mg/litre standard solution that is the variable concentrations of 0～10 micrograms per litre, measure the typical curve that obtains lead with hydride generation-atomic spectroscopy, this process comprises that current-carrying carries standard solution and reacts with reductive agent to the reaction block place, generate the hydride of the lead of gaseous state, the alanate of gaseous state is delivered to atomization in the atomizer by carrier gas then, record corresponding spectral signal with atomic spectroscopy, just can obtain plumbous typical curve with concentration of standard solution and spectral signal mapping; The 3rd step sample determination, use hydride generation method-atomic spectroscopy working sample liquid to be measured, this process comprises that current-carrying carries sample liquid to be measured and reacts with reductive agent to the reaction block place, generate the hydride of the lead of gaseous state, the alanate of gaseous state is delivered to atomization in the atomizer by carrier gas then, record corresponding spectral signal with atomic spectroscopy, more quantitative with typical curve.
2. the method for measurement blood lead according to claim 1 is characterized in that: the component of described reductive agent is potassium borohydride or sodium borohydride, the potassium ferricyanide of 10 grams per liters-30 grams per liter and the weak acid of 5 grams per liters-20 grams per liter of the NaOH of 10 grams per liters-30 grams per liter or potassium hydroxide, 5 grams per liters-30 grams per liter.
3. the method for measurement blood lead according to claim 2 is characterized in that: described weak acid is tartrate, oxalic acid or boric acid.
4. according to the method for claim 1 or 2 or 3 described measurement blood leads, it is characterized in that: described current-carrying is a kind of mixed solution, wherein contains percent by volume and be the mixed solution of the oxidizing agent solution of 1.0%～4.5% inorganic acid and volume or mass percent 1.0～5.0%.
5. the method for measurement blood lead according to claim 4 is characterized in that: described inorganic acid is hydrochloric acid, nitric acid, perchloric acid or sulfuric acid;
6. the method for measurement blood lead according to claim 5 is characterized in that: described oxidizing agent solution is hydrogen peroxide, potassium persulfate.
7. the ultraviolet assisted extraction instrument of the glimmering measurement blood lead of hydride generation atom is characterized in that: comprise lighttight housing, be provided with an above uviol lamp (1) in housing, the one side of lamp or be provided with the container of depositing sample all around.
8. ultraviolet assisted extraction instrument according to claim 7 is characterized in that: described container is the sample hose (2) that is placed on the support.
9. ultraviolet assisted extraction instrument according to claim 7 is characterized in that described container is the processing pipeline (3) that is coiled on the uviol lamp.
10 ultraviolet assisted extraction instrument according to claim 9 is characterized in that the two ends of described processing pipeline are provided with stop valve (4).
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| CNB2006100764504A CN100541199C (en) | 2006-04-25 | 2006-04-25 | Ultraviolet assisted extraction hydride generation atomic spectroscopy is surveyed the method for blood lead |
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| CNB2006100764504A CN100541199C (en) | 2006-04-25 | 2006-04-25 | Ultraviolet assisted extraction hydride generation atomic spectroscopy is surveyed the method for blood lead |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100573109C (en) * | 2007-05-31 | 2009-12-23 | 中国铝业股份有限公司 | The plumbous assay method of trace in a kind of aluminium ingot |
| CN102564837A (en) * | 2010-12-20 | 2012-07-11 | 北京吉天仪器有限公司 | Novel ultraviolet preprocessing device |
| CN102680455A (en) * | 2011-03-14 | 2012-09-19 | 浙江省农业科学院 | Medium acidity control mathematical model for determining lead by using atomic fluorescence method |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20130270996A1 (en) * | 2010-12-20 | 2013-10-17 | Beijing Titan Instruments Co., Ltd. | Ultraviolet Pretreatment Device |
-
2006
- 2006-04-25 CN CNB2006100764504A patent/CN100541199C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100573109C (en) * | 2007-05-31 | 2009-12-23 | 中国铝业股份有限公司 | The plumbous assay method of trace in a kind of aluminium ingot |
| CN102564837A (en) * | 2010-12-20 | 2012-07-11 | 北京吉天仪器有限公司 | Novel ultraviolet preprocessing device |
| CN102680455A (en) * | 2011-03-14 | 2012-09-19 | 浙江省农业科学院 | Medium acidity control mathematical model for determining lead by using atomic fluorescence method |
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| CN100541199C (en) | 2009-09-16 |
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