CN108195984A - Multivitamin detection method and detecting system in a kind of dry blood cake - Google Patents

Multivitamin detection method and detecting system in a kind of dry blood cake Download PDF

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Publication number
CN108195984A
CN108195984A CN201711481553.3A CN201711481553A CN108195984A CN 108195984 A CN108195984 A CN 108195984A CN 201711481553 A CN201711481553 A CN 201711481553A CN 108195984 A CN108195984 A CN 108195984A
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blood cake
extract liquor
dry blood
cleaned
dry
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林芸
张旭光
贺瑞坤
肖健
汪玉芳
彭辉
叶少文
苏昭仑
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BY Health Co Ltd
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BY Health Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/88Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/06Preparation

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  • Life Sciences & Earth Sciences (AREA)
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  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
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  • Investigating Or Analysing Biological Materials (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)

Abstract

The invention belongs to multivitamin detection method and detecting systems in the technical field of blood testing more particularly to a kind of dry blood cake.The present invention provides multivitamin detection methods in a kind of dry blood cake, include the following steps:S101:Internal standard compound, dry blood cake after being handled are added in dry blood cake;S102:Blood cake dry after processing with the first extract liquor is extracted, obtain the first detection liquid or extracts blood cake dry after processing with the second extract liquor, obtains the second detection liquid;S103:The described first detection liquid or the second detection liquid are detected using liquid chromatography mass combined instrument;Wherein, first extract liquor is the methanol aqueous solution that percent by volume is 5% 95%;Second extract liquor is 10 90% methanol aqueous solution.Multivitamin in the detection method energy short time of the present invention in detection micro blood, solution detect technological deficiency time-consuming and laborious in multivitamin method at present.

Description

Multivitamin detection method and detecting system in a kind of dry blood cake
Technical field
The invention belongs to multivitamin detection methods in the technical field of blood testing more particularly to a kind of dry blood cake And detecting system.
Background technology
The vniims method of currently used detection human body is detected using blood plasma, and plasma sample is passed through sodium hydroxide alkali Upper machine is measured after change, protein precipitation and petroleum ether extraction concentration, however, what the vitamin detection method of the prior art needed Blood is more, and blood preseration transporter noodles part is harsh, and can only detect single vitamin content every time, a variety of for detecting During vitamin, the detection method of the prior art is very time-consuming and laborious.
Invention content
In view of this, the present invention provides multivitamin detection method and detecting system in a kind of dry blood cake, can have Effect solves to detect technological deficiency time-consuming and laborious in multivitamin method at present.
The present invention also provides multivitamin detection methods in a kind of dry blood cake, include the following steps:
S101:Internal standard compound, dry blood cake after being handled are added in dry blood cake;
S102:Blood cake dry after processing is extracted with the first extract liquor, dry blood after obtaining the first detection liquid or handling Spot is extracted with the second extract liquor, obtains the second detection liquid;
S103:The described first detection liquid or the second detection liquid are detected using liquid chromatograph-mass spectrometer;
Wherein, first extract liquor is the methanol aqueous solution that percent by volume is 5%-95%;Second extract liquor Methanol aqueous solution for 10-90%.
More preferably, first extract liquor is the methanol aqueous solution that percent by volume is 70%;Second extract liquor For 20% methanol aqueous solution
It should be noted that the first extract liquor is used to extract fat-soluble vitamin;Second extract liquor is water-soluble for extracting The vitamin of property.
Preferably, the internal standard compound is specially Isotopic Internal Standard liquid, the Isotopic Internal Standard liquid 5-40 μ L.
More preferably, the 5 μ L of Isotopic Internal Standard liquid.
Preferably, the internal standard compound is thiamines-(- 5 base -13C3 of 4- methyl-1 3C- thiazoles) hydrochloride, riboflavin (13C4,99%;15N2,98%), niacinamide -2,4,5,6-d4,25- hydroxyl ergosterols d3 (6,19,19-D3,97%), dimension life Plain B5 (two-Beta-alanine -13C6,15N2) calcium salt, alpha-tocopherol-(ring -5,7- dimethyl-d6), pyridoxal/vitamin B6 It is one or more in (vitamin B6) (methyl D 3,98%) and alltrans retinol d5.
More preferably, thiamines-(4- methyl-1 3C- thiazole -5- bases -13C3) hydrochloride uses a concentration of 100ng/ml, core Flavine (13C4,99%;15N2,98%) a concentration of 20ng/ml, niacinamide -2,4 are used, 5,6-d4 use a concentration of 1000ng/ Ml, 25- hydroxyl ergosterol d3 (6,19,19-D3,97%) using a concentration of 20ng/ml, vitamin B5 (two-Beta-alanine- 13C6,15N2) calcium salt using a concentration of 200ng/ml, alpha-tocopherol-(ring -5,7- dimethyl-d6) using a concentration of 10000ng/ml, pyridoxal/vitamin B6 (vitamin B6) (methyl D 3,98%) are regarded using a concentration of 100ng/ml, alltrans Flavol d5 uses a concentration of 1000ng/ml.
Preferably, first extract liquor is 5-100 μ L, the extraction flow velocity of first extract liquor is 10-150 μ L/ ml。
More preferably, first extract liquor is 20 μ L, the extraction flow velocity of first extract liquor is 50 μ L/ml.
Preferably, second extract liquor is 5-100 μ L, the extraction flow velocity of second extract liquor is 10-150 μ L/ ml。
More preferably, second extract liquor is 20 μ L, the extraction flow velocity of second extract liquor is 50 μ L/ml.
Preferably, the S101 is further included:Processing, drying time 1-60s is dried in blood cake dry after processing.
More preferably, the drying time is 5s.
The present invention also provides multivitamin automatic checkout system in a kind of dry blood cake, including:Pretreatment unit, extraction Take unit and detection unit;
The pretreatment unit is used to add in internal standard compound, dry blood cake after being handled to dry blood cake;
The extraction cells are extracted for dry blood cake after handling with the first extract liquor, obtain the first detection liquid or Blood cake dry after processing with the second extract liquor is extracted, obtains the second detection liquid;
The detection unit to described first detection liquid or it is described second detection liquid using liquid chromatograph-mass spectrometer into Row detection.
Preferably, it further includes:Cleaning unit is used to clean the extraction cells.
Preferably, when the extraction cells are extracted using the first extract liquor, cleaning unit is specially to the extraction The outlet of unit is taken to carry out wash cycles using the first extract liquor, cleaning solution and the first extract liquor, the wash cycles program is:
S201:The outlet of the extraction cells is cleaned using first extract liquor, to clean for the first time;
S202:The outlet of extraction cells after being cleaned to first time is cleaned using the cleaning solution, is cleaned for second;
S203:The outlet of extraction cells after being cleaned to second is cleaned using first extract liquor, clear for third time It washes;
The import of the extraction cells carries out single cleaning using the first extract liquor.
More preferably, the scavenging period of S201 cleanings for the first time is 5-200s.
More preferably, the scavenging period of S201 cleanings for the first time is 30s.
More preferably, second of scavenging period cleaned of the S202 is 5-200s.
More preferably, second of scavenging period cleaned of the S202 is 30s.
More preferably, the scavenging period of the S203 third times cleaning is 5-200s.
More preferably, the scavenging period of the S203 third times cleaning is 30s.
More preferably, the scavenging period of the first extract liquor single cleaning is 5-200s.
More preferably, the scavenging period of the first extract liquor single cleaning is 20s.
Preferably, when the extraction cells are extracted using the second extract liquor, cleaning unit is specially to the extraction The outlet of unit is taken to carry out wash cycles using the second extract liquor, cleaning solution and the second extract liquor, the wash cycles program is:
S301:The outlet of the extraction cells is cleaned using second extract liquor, to clean for the first time;
S302:The outlet of extraction cells after being cleaned to first time is cleaned using the cleaning solution, is cleaned for second;
S303:The outlet of extraction cells after being cleaned to second is cleaned using second extract liquor, clear for third time It washes;
The import of the extraction cells carries out single cleaning using the second extract liquor.
More preferably, the scavenging period of S301 cleanings for the first time is 5-200s.
More preferably, the scavenging period of S301 cleanings for the first time is 30s.
More preferably, second of scavenging period cleaned of the S302 is 5-200s.
More preferably, second of scavenging period cleaned of the S302 is 30s.
More preferably, the scavenging period of the S303 third times cleaning is 5-200s.
More preferably, the scavenging period of the S303 third times cleaning is 30s.
More preferably, the scavenging period of the single cleaning of second extract liquor is 5-200s.
More preferably, the scavenging period of the single cleaning of second extract liquor is 20s.
Preferably, the cleaning solution is specially acetone:Isopropanol:Methanol:The mixed liquor of water, wherein, the acetone:Institute State isopropanol:The methanol:The volume ratio of the water is 1:1:1:1.
Dry blood cake (driedblood spots, DBS) sampling method, earliest by Robert Guthrie 1963 propose, The positions such as finger tip, ear-lobe or heel are pricked by using disposable blood taking needle, drop in pipette, extract blood or directly filter The method sampled on paper.Compared to conventional biological sample collection mode, dry blood cake method of sampling wound is small, passes through foot more With, toe, finger take blood, sampling is very convenient.The present invention develops multivitamin detection method in a kind of dry blood cake, from Multivitamin is accurately detected in the micro blood of dry blood cake.The detection method very simple of the present invention and quick, including S101: Internal standard compound, dry blood cake after being handled are added in dry blood cake;S102:Blood cake dry after processing is extracted with the first extract liquor, It obtains the first detection liquid or extracts blood cake dry after processing with the second extract liquor, obtain the second detection liquid;S103:Using Liquid chromatograph-mass spectrometer is detected the first detection liquid or the second detection liquid;Wherein, first extract liquor is volume Percentage is the methanol aqueous solution of 5%-95%;Methanol aqueous solution of second extract liquor for 10%-90%, the present invention first Extract liquor and the second extraction liquid energy extract multivitamin from micro blood, and three steps will detect a variety of in dry blood cake Vitamin and its testing result correlation and repeatability height, meanwhile, the present invention also provides a kind of automatic checkout system to dry blood Spot realizes full-automatic extraction, avoids the possibility for occurring mistake in artificial extraction process, greatly improves weighing for extraction efficiency Renaturation, moreover it is possible to realize the high throughput analysis of sample.
Description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, to embodiment or will show below There is attached drawing needed in technology description to be briefly described.
Fig. 1 shows vitamin A standard curve;
Fig. 2 shows vitamin D standard curve;
Fig. 3 shows vitamin E standard curve;
Fig. 4 shows vitamin B1 standard curve;
Fig. 5 shows vitamin B2 standard curve;
Fig. 6 shows vitamin B3 standard curve;
Fig. 7 shows vitamin B5 standard curve;
Fig. 8 shows vitamin B6 standard curve;
Fig. 9 shows Vitamin B9 standard curve;
Figure 10 shows dry blood cake detection method using the present invention and the inspection using conventional new blood vitamin detection method Survey the result correlation analysis of vitamin A;
Figure 11 shows dry blood cake detection method using the present invention and the inspection using conventional new blood vitamin detection method Survey the result correlation analysis of vitamin D;
Figure 12 shows dry blood cake detection method using the present invention and the inspection using conventional new blood vitamin detection method Survey the result correlation analysis of vitamin E;
Figure 13 shows dry blood cake detection method using the present invention and the inspection using conventional new blood vitamin detection method Survey the result correlation analysis of vitamin B1;
Figure 14 shows dry blood cake detection method using the present invention and the inspection using conventional new blood vitamin detection method Survey the result correlation analysis of vitamin B2;
Figure 15 shows dry blood cake detection method using the present invention and the inspection using conventional new blood vitamin detection method Survey the result correlation analysis of vitamin B3;
Figure 16 shows dry blood cake detection method using the present invention and the inspection using conventional new blood vitamin detection method Survey the result correlation analysis of vitamin B5;
Figure 17 shows dry blood cake detection method using the present invention and the inspection using conventional new blood vitamin detection method Survey the result correlation analysis of vitamin B6;
Figure 18 shows dry blood cake detection method using the present invention and the inspection using conventional new blood vitamin detection method Survey the result correlation analysis of Vitamin B9.
Specific embodiment
The present invention provides multivitamin detection method and detecting system in a kind of dry blood cake, the present invention can be examined quickly The multivitamin in human body is surveyed, effectively solves existing time-consuming and laborious technological deficiency during detection multivitamin at present.
The technical solution in the embodiment of the present invention will be clearly and completely described below, it is clear that described implementation Example is only part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common Technical staff's all other embodiments obtained without making creative work belong to the model that the present invention protects It encloses.
Wherein, the raw material of following embodiment is commercially available or self-control.
It should be noted that the correspondence of targeted vitamins and target compound is as shown in Table 1 and Table 2.
1 fat-soluble targeted vitamins of table and target compound
Targeted vitamins Target compound
Vitamin A Retinol (reitnol)
Vitamin D Dihydroxy calciferol (2,5-hydroxycholcalciferol)
Vitamin E Alpha-tocopherol (alpha-tocopherol)
The water-soluble targeted vitamins of table 2 and target compound
Targeted vitamins Target compound
Vitamin B1 Diphosphothiamine (thiamine diphosphate)
Vitamin B2 Riboflavin (riboflavin)
Vitamin B3 Niacinamide (nicotinamide)
Vitamin B5 Pantothenic acid (pantothenicacid)
Vitamin B6 Pyridoxol (pyridoxine)
Vitamin B9 Folic acid (folic acid)
Japanese Shimadzu Nexera UHPLC Ultra Performance Liquid Chromatography instruments, American AB Sciex4500 triple four The compound mass spectrograph of pole bar-linear ion hydrazine
Embodiment 1
The present embodiment is to detect liposoluble vitamin in dry blood cake using the detection method of the present invention, the specific steps are:
1st, dry blood cake card sample is prepared:By fresh blood drop on special dry blood cake card, the blood volume of new blood is 25 μ L, are protected from light dry 2h.
2nd, the dry blood cake of step 1 is transferred in pretreatment unit using software, to dry blood cake sprinkling 5 in pretreatment unit μ L Isotopic Internal Standard liquid;After dry 5s, dry blood cake after being handled.
3rd, blood cake dry after processing is transferred in extraction cells using software, target in dry blood cake is extracted with 20 μ L extract liquors Liposoluble vitamin.After extraction, cleaning unit prepares to extract next dry blood cake after automatically cleaning extraction cells. Specifically cleaning process is:S201:The outlet of extraction cells is cleaned using the first extract liquor, to clean for the first time;S202:To The outlet of extraction cells after primary cleaning is cleaned using cleaning solution, is cleaned for second;S203:Extraction after being cleaned to second The outlet of unit is taken to be cleaned using the first extract liquor, is cleaned for third time;The import of extraction cells is carried out using the first extract liquor Single cleans.Internal standard solution, extraction process and cleaning process parameter see the table below 3.
3 parameter list of table
4th, the first detection liquid (20 μ L contain target compound extract liquor in blood) of extraction cells is input by inspection by software It surveys unit and carries out liquid chromatograph-mass spectrometer detection.Liquid chromatograph parameter setting sees below list lattice;Mass spectrometer ion source is joined Number setting sees below list lattice;Target compound MRM parameter settings see below list lattice.
4 parameter list of table
5 parameter list of table
Table 6
5th, interpretation of result:Liposoluble vitamin retention time, detection limit (LOD) and quantitative limit (LOQ such as tables 7.
7 parameter list of table
It please refers to Fig.1 to Fig.3, Fig. 1 to Fig. 3 (has marked regression equation and phase relation for liposoluble vitamin standard curve Number R2)
According to diagram, the equal display target compound standard curve tool of related coefficient of vitamin A. D. E standard curve is preferable It is linear.
Embodiment 2
The present embodiment is liposoluble vitamin stability test (RSD), and method is as follows:
6 dry blood cakes are made using same Fresh blood sample in experiment, and continuous extraction sample introduction is with this determining dry blood cake The stability of vitamin detection method, the results are shown in Table 8, and as known from Table 8, the fat-soluble dimension life in dry blood cake is tested in this implementation Element has good stability.
8 liposoluble vitamin stability data of table
rep1 rep2 rep3 rep4 rep5 rep6 RSD (%)
Vitamin A 53543 59194 48479 51760 53715 54267 6.5
Vitamin D 65905 65251 60741 59389 67451 64248 4.9
Vitamin E 157640 166970 169310 189440 165480 193970 8.3
Embodiment 3
The present embodiment is to detect water soluble vitamin in dry blood cake using the detection method of the present invention, the specific steps are:
1st, dry blood cake card sample is prepared:By fresh blood drop on special dry blood cake card, the blood volume of new blood is 25 μ L, are protected from light dry 2h.
2nd, the dry blood cake of step 1 is transferred in pretreatment unit using software, to dry blood cake sprinkling 5 in pretreatment unit μ L Isotopic Internal Standard liquid;After dry 5s, dry blood cake after being handled.
3rd, blood cake dry after processing is transferred in extraction cells using software, target in dry blood cake is extracted with 20 μ L extract liquors Liposoluble vitamin.After extraction, cleaning unit prepares to extract next dry blood cake after automatically cleaning extraction cells. Specifically cleaning process is:S301:The outlet of extraction cells is cleaned using the second extract liquor, to clean for the first time;S302:To The outlet of extraction cells after primary cleaning is cleaned using cleaning solution, is cleaned for second;S303:Extraction after being cleaned to second The outlet of unit is taken to be cleaned using the second extract liquor, is cleaned for third time;The import of extraction cells is carried out using the second extract liquor Single cleans.Internal standard solution, extraction process and cleaning process parameter see the table below 8.
9 parameter list of table
4th, it is controlled by software the second detection liquid (20 μ L contain target compound extract liquor in blood) of extraction cells is defeated Liquid chromatograph-mass spectrometer detection is carried out into detection unit.Liquid chromatograph parameter setting sees below list lattice;Mass spectrograph ion Source parameter setting sees below list lattice;Target compound MRM parameter settings see below list lattice.
10 parameter list of table
11 parameter list of table
12 parameter list of table
5th, interpretation of result:(LOQ is as shown in table 12 for liposoluble vitamin retention time, detection limit (LOD) and quantitative limit.
13 liposoluble vitamin retention time of table, detection limit (LOD) and quantitative limit (LOQ)
Fig. 4 to Fig. 9 is please referred to, Fig. 4 to Fig. 9 (has marked regression equation and phase relation for water soluble vitamin standard curve Number R2) vitamin B1, the related coefficient equal display target compound standard curve tool of B2, B3, B5, B6, B9 standard curve be preferable It is linear.
Embodiment 4
The present embodiment is water soluble vitamin stability test (RSD), and method is as follows:
6 dry blood cakes are made using same Fresh blood sample in experiment, and continuous extraction sample introduction is with this determining dry blood cake The stability of vitamin detection method, as a result as shown in table 13, as known from Table 13, the water soluble vitamin in dry blood cake is tested in this implementation Raw element has good stability.
14 water soluble vitamin stability data of table
rep1 rep2 rep3 rep4 rep5 rep6 RSD (%)
Vitamin B1 4426 3957 4512 4466 4358 4679 5.5
Vitamin B2 3799 4015 4198 4057 3658 3974 4.9
Vitamin B3 31475000 34597000 32597000 36041000 34597000 32479000 5.1
Vitamin B5 432510 478510 467910 459710 451020 461010 3.4
Vitamin B6 1101500 1248900 1104400 1315000 1278100 1161400 7.6
Vitamin B9 116552 117591 121798 102798 115467 120549 5.9
Embodiment 5
The present embodiment is dry blood cake detection method using the present invention with using conventional new blood vitamin detection method Comparison embodiment, experimentation is:Using same Fresh blood sample, conventional manual is being used to extract and is being examined with liquid chromatography mass spectrometric Measured data simultaneously, makes a dry blood cake card and determines targeted vitamins concentration using the dry blood cake detection method of the present invention. Two groups of data are subjected to correlation analysis, two groups of data dependences are shown in Figure 10 to Figure 18, from related coefficient as can be seen that two kinds of inspections Result obtained by survey method has stronger correlation, therefore, the testing result of dry blood cake detection method of the invention, precision with Conventional new blood vitamin detection method is similar, but the dry blood cake detection method of the present invention can detect multivitamin simultaneously, It is time saving and energy saving.
In conclusion conventional new blood vitamin detection method needs the new blood of 200 μ L, transported in the preservation of sample Defeated aspect condition is harsh, and detection method is very cumbersome, and compared with conventional new blood vitamin detection method, of the invention is dry Blood cake detection method has a clear superiority, and dry blood cake card is protected from light at shady and cool drying after blood sampling and preserves, and transportation cost is low (only It need to be protected from light in packaging in sealing and add in drier, antioxidant).Conventional new blood vitamin detection method needs 200 μ L's New blood, and the dry blood cake detection method of the present invention need to only take the new blood of 15 μ L, blood sampling volume is lower.It is conventional new Fresh blood vitamin detection method labor intensive, and the dry blood cake detection method of the present invention realizes full-automatic extraction, avoids artificial Occur the possibility of mistake in extraction process, greatly improve the repeatability of extraction efficiency.Conventional new blood vitamin inspection Survey method takes longer, and the time cost of dry blood cake detection method of the present invention is only used for liquid phase mass spectrometric analysis, is analyzing While dry blood cake extraction platform carry out extraction operation, be equivalent to zero-time cost, can realize high throughput sample analysis (hundreds of Sample extracts detection simultaneously, and night does not stop work operation).
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications also should It is considered as protection scope of the present invention.

Claims (10)

1. multivitamin detection method in a kind of dry blood cake, which is characterized in that include the following steps:
S101:Internal standard compound, dry blood cake after being handled are added in dry blood cake;
S102:Blood cake dry after processing is extracted with the first extract liquor, dry blood cake is used after obtaining the first detection liquid or handling Second extract liquor is extracted, and obtains the second detection liquid;
S103:The described first detection liquid or the second detection liquid are detected using liquid chromatograph-mass spectrometer;
Wherein, first extract liquor is the methanol aqueous solution that percent by volume is 5%-95%;Second extract liquor is 10- 90% methanol aqueous solution.
2. multivitamin detection method in dry blood cake according to claim 1, which is characterized in that the internal standard compound tool Body be Isotopic Internal Standard liquid, the Isotopic Internal Standard liquid 5-40 μ L.
3. multivitamin detection method in dry blood cake according to claim 1, which is characterized in that first extraction Liquid is 5-100 μ L, and the extraction flow velocity of first extract liquor is 10-150 μ L/ml.
4. multivitamin detection method in dry blood cake according to claim 1, which is characterized in that second extraction Liquid is 5-100 μ L, and the extraction flow velocity of second extract liquor is 10-150 μ L/ml.
5. multivitamin detection method in dry blood cake according to claim 1, which is characterized in that the S101 is also wrapped It includes:Processing, drying time 1-60s is dried in blood cake dry after processing.
6. a kind of multivitamin automatic checkout system in dry blood cake, which is characterized in that including:Pretreatment unit, extraction are single Member and detection unit;
The pretreatment unit is used to add in internal standard compound, dry blood cake after being handled to dry blood cake;
The extraction cells are used for dry blood cake after handling and are extracted with the first extract liquor, obtain the first detection liquid or will locate Dry blood cake is extracted with the second extract liquor after reason, obtains the second detection liquid;
The detection unit examines the described first detection liquid or the second detection liquid using liquid chromatograph-mass spectrometer It surveys.
7. multivitamin automatic checkout system in dry blood cake according to claim 6, which is characterized in that further include: Cleaning unit, the cleaning unit are used to clean the extraction cells.
8. multivitamin automatic checkout system in dry blood cake according to claim 7, which is characterized in that the extraction When unit is extracted using the first extract liquor, cleaning unit is specially that the outlet to the extraction cells is extracted using first Liquid, cleaning solution and the first extract liquor carry out wash cycles, and the wash cycles program is:
S201:The outlet of the extraction cells is cleaned using first extract liquor, to clean for the first time;
S202:The outlet of extraction cells after being cleaned to first time is cleaned using the cleaning solution, is cleaned for second;
S203:The outlet of extraction cells after being cleaned to second is cleaned using first extract liquor, is cleaned for third time;
The import of the extraction cells carries out single cleaning using the first extract liquor.
9. multivitamin automatic checkout system in dry blood cake according to claim 7, which is characterized in that the extraction When unit is extracted using the second extract liquor, cleaning unit is specially that the outlet to the extraction cells is extracted using second Liquid, cleaning solution and the second extract liquor carry out wash cycles, and the wash cycles program is:
S301:The outlet of the extraction cells is cleaned using second extract liquor, to clean for the first time;
S302:The outlet of extraction cells after being cleaned to first time is cleaned using the cleaning solution, is cleaned for second;
S303:The outlet of extraction cells after being cleaned to second is cleaned using second extract liquor, is cleaned for third time;
The import of the extraction cells carries out single cleaning using the second extract liquor.
10. multivitamin automatic checkout system in dry blood cake according to claim 8 or claim 9, which is characterized in that described Cleaning solution is specially acetone:Isopropanol:Methanol:The mixed liquor of water, wherein, the acetone:The isopropanol:The methanol:Institute The volume ratio for stating water is 1:1:1:1.
CN201711481553.3A 2017-12-29 2017-12-29 Multivitamin detection method and detecting system in a kind of dry blood cake Pending CN108195984A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110146628A (en) * 2019-06-18 2019-08-20 上海可力梅塔生物医药科技有限公司 A kind of high performance liquid chromatography string mass-spectrometric technique detects the kit of folic acid in blood cake
CN110146626A (en) * 2019-06-18 2019-08-20 上海可力梅塔生物医药科技有限公司 A kind of method of folic acid in high performance liquid chromatography string mass Spectrometry for Determination blood cake
CN110174476A (en) * 2019-06-10 2019-08-27 合肥谱佳医学检验实验室有限公司 The detection method of the Liquid Chromatography-Tandem Mass Spectrometry of a variety of liposoluble vitamins in a kind of dried blood spot
US10656059B2 (en) 2018-03-07 2020-05-19 Alcala Pharmaceutical, Inc. Method for qualitative and quantitative multiplexing of drug analytes from biological samples
CN114527230A (en) * 2022-02-28 2022-05-24 上海药明奥测医疗科技有限公司 Method for detecting concentration of vitamin A and vitamin E in human dry blood spots
CN114755323A (en) * 2022-03-24 2022-07-15 北京和合医学诊断技术股份有限公司 Method and kit for detecting content of fat-soluble vitamins in dried blood paper
CN115343379A (en) * 2022-04-20 2022-11-15 杭州谱聚医疗科技有限公司 Preparation method of blank blood matrix and standard substance and detection method of vitamin

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6451611B1 (en) * 2000-07-28 2002-09-17 Statens Serum Institute Quantitative analysis of hexose-monophosphates from biological samples
US8729463B2 (en) * 2010-03-29 2014-05-20 Waters Technologies Corporation Measurement of 25-hydroxyvitamin D3 and C3-epi-25-hydroxyvitamin D3
WO2014150900A1 (en) * 2013-03-15 2014-09-25 Baylor Research Institute Methods and compositions for enhanced analyte detection from blood
CN104914176A (en) * 2015-05-08 2015-09-16 重庆医科大学附属儿童医院 Method for quantitatively analyzing retinol and precursor thereof on dry blood spot card with tiny amount of blood
CN106770802A (en) * 2017-02-23 2017-05-31 广州市丰华生物工程有限公司 It is a kind of to detect multivitamin method and kit in dry blood spot simultaneously

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6451611B1 (en) * 2000-07-28 2002-09-17 Statens Serum Institute Quantitative analysis of hexose-monophosphates from biological samples
US8729463B2 (en) * 2010-03-29 2014-05-20 Waters Technologies Corporation Measurement of 25-hydroxyvitamin D3 and C3-epi-25-hydroxyvitamin D3
WO2014150900A1 (en) * 2013-03-15 2014-09-25 Baylor Research Institute Methods and compositions for enhanced analyte detection from blood
CN104914176A (en) * 2015-05-08 2015-09-16 重庆医科大学附属儿童医院 Method for quantitatively analyzing retinol and precursor thereof on dry blood spot card with tiny amount of blood
CN106770802A (en) * 2017-02-23 2017-05-31 广州市丰华生物工程有限公司 It is a kind of to detect multivitamin method and kit in dry blood spot simultaneously

Non-Patent Citations (5)

* Cited by examiner, † Cited by third party
Title
GÖTZ SCHLOTTERBECK 等: "Automated dried blood spot instrumentation coupled to HPLC-QqQ mass spectrometry – A vitamin D and E case study", 《IMSC 2014 20TH INTERNATIONAL MASS SPECTROMETRY CONFERENCE PROVISIONAL ABSTRACT BOOK》 *
PAUL ABU-RABIE 等: "Dried matrix spot direct analysis: evaluating the robustness of a direct elution technique for use in quantitative bioanalysis", 《BIOANALYSIS》 *
U. DUTHALER 等: "Automated high throughput analysis of antiretroviral drugs in dried blood spots", 《J. MASS SPECTROM.》 *
郭建博 等: "超高效液相色谱法快速测定复合维生素产品中的10 种水溶性维生素", 《食品安全质量检测学报》 *
韩吉春 等: "液相色谱-串联质谱法检测干血点样本中25-羟基维生素D2和25-羟基维生素D3", 《分析化学》 *

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10656059B2 (en) 2018-03-07 2020-05-19 Alcala Pharmaceutical, Inc. Method for qualitative and quantitative multiplexing of drug analytes from biological samples
US11054349B2 (en) 2018-03-07 2021-07-06 Alcala Pharmaceutical, Inc. Method for preparation of dried blood sample for multiplexing of analytes
CN110174476A (en) * 2019-06-10 2019-08-27 合肥谱佳医学检验实验室有限公司 The detection method of the Liquid Chromatography-Tandem Mass Spectrometry of a variety of liposoluble vitamins in a kind of dried blood spot
CN110146628A (en) * 2019-06-18 2019-08-20 上海可力梅塔生物医药科技有限公司 A kind of high performance liquid chromatography string mass-spectrometric technique detects the kit of folic acid in blood cake
CN110146626A (en) * 2019-06-18 2019-08-20 上海可力梅塔生物医药科技有限公司 A kind of method of folic acid in high performance liquid chromatography string mass Spectrometry for Determination blood cake
CN114527230A (en) * 2022-02-28 2022-05-24 上海药明奥测医疗科技有限公司 Method for detecting concentration of vitamin A and vitamin E in human dry blood spots
CN114755323A (en) * 2022-03-24 2022-07-15 北京和合医学诊断技术股份有限公司 Method and kit for detecting content of fat-soluble vitamins in dried blood paper
CN115343379A (en) * 2022-04-20 2022-11-15 杭州谱聚医疗科技有限公司 Preparation method of blank blood matrix and standard substance and detection method of vitamin

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