CN110361490A - The pre-treating method of Nitrofuran metatolites - Google Patents
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- G—PHYSICS
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- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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Abstract
The present invention relates to the pre-treating methods of Nitrofuran metatolites, belong to the technical field of Nitrofuran metatolites detection comprising 1. following steps: S1: cleaning sample, blends sample and obtains sample；S2: hydrochloric acid and derivatization reagent, the ultrasound 1-1.5h at a temperature of 50-65 DEG C are added into sample；S3: adjusting PH to 7.4, and hexamethylene, neutral alumina is added and promotees layering agent, refrigerated centrifuge after shaking obtains bottom solid phase, middle layer water phase A, top layer organic phase；S4: it takes middle layer water phase A to carry out Solid Phase Extraction, then obtains eluent B with eluent；S5: eluent B is dried with nitrogen, mobile phase constant volume when initial.The present invention has the effect of keeping the Nitrofuran metatolites pretreatment process time shorter.
Description
Technical field
The present invention relates to the technical fields of Nitrofuran metatolites detection, more particularly, to Nitrofuran metatolites
Pre-treating method.
Background technique
Nitrofuran metabolites are a kind of artificial synthesized broad-spectrum antibiotics at present, because price is lower and effect is good, and
It is widely used in livestock and poultry and culture fishery, since Nitrofuran metabolites and its metabolin have carcinogenic, teratogenicity pair to human body
Effect, some countries have forbidden Nitrofuran metabolites to use in livestock and poultry and aquatic livestock food, still, itrofurans
Prototype medicine is metabolized rapidly in vivo, can not be detected, but its metabolite because with protein in conjunction with due to guarantee long-time stable
In the presence of.So generally using nitrofurans medicament metabolite as the detection of target analytes, to reach detection nitrofuran
The purpose of object residual quantity.
There are many detection method of existing Nitrofuran metatolites, such as the method in GB/T20752-2006, for flesh
Meat, internal organ, fish and shrimp are substantially following steps: hydrolysis and derivatization: methanol-water mixed solution (volume being added in the sample
Than 2:1) it washs, in residue plus hydrochloric acid, internal standard standard solution, o-nitrobenzaldehyde, mixing are protected from light at 37 DEG C and shake hydrolysis
16h；Extraction and concentration: taking out sample, be cooled to room temperature, and potassium phosphate,monobasic is added, and with sodium hydroxide tune PH to 7.4, it is solid to cross HLB
Phase extraction column, is eluted with ethyl acetate, is dried with nitrogen eluent, is obtained pre-treatment sample, is then measured.
Prior art among the above has the following deficiencies: that derivatization process needs are protected from light concussion hydrolysis 16h at 37 DEG C,
Keep the Nitrofuran metatolites pretreatment process time long.
Summary of the invention
The purpose of the present invention one, which is to provide, a kind of makes Nitrofuran metatolites pretreatment process time shorter nitro furan
It mutters the pre-treating method of metabolite.
Above-mentioned purpose of the invention has the technical scheme that
The pre-treating method of Nitrofuran metatolites, comprising the following steps:
S1: cleaning sample, blends sample and obtains sample；
S2: hydrochloric acid and derivatization reagent, the ultrasound 1-1.5h at a temperature of 50-65 DEG C are added into sample；
S3: adjusting PH to 7.4, and hexamethylene, neutral alumina is added and promotees layering agent, it is solid to obtain bottom for refrigerated centrifuge after shaking
Phase, middle layer water phase A, top layer organic phase；
S4: it takes middle layer water phase A to carry out Solid Phase Extraction, then obtains eluent B with eluent；
S5: eluent B is dried with nitrogen, mobile phase constant volume when initial.
By using above-mentioned technical proposal, in animal body, the form of Nitrofuran metatolites one reference states of the overwhelming majority
In conjunction with protein, sample is blended, the relative contact product of the hydrochloric acid and derivatization reagent that make sample and subsequent addition is larger,
The Nitrofuran metatolites in sample in conjunction with protein are enable preferably to separate in acidic environment with protein, from
And highest Nitrofuran metatolites residual quantity is obtained from sample, meanwhile, hydrolysing step under hydrochloric acid acidulated condition with spread out
It gives birth to while carrying out, so that the Nitrofuran metatolites in sample is had longer time and Separation of Proteins, ensure that nitro
The fractional dose of furans metabolite；It is reacted with the free state Nitrofuran metatolites that Separation of Proteins is opened with derivatization reagent,
Increase the molecular weight of the derivative of Nitrofuran metatolites, is convenient for qualitative detection.
The temperature of derivatization and the setting of ultrasound condition accelerate the separation speed of Nitrofuran metatolites and protein
Degree, and be conducive to accelerate derivatization speed, reduce the time of derivatization, to be conducive to Nitrofuran metatolites pre-treatment
Process time reduces.
The addition of hexamethylene, fat can incorporate in hexamethylene, and the water layer where hexamethylene and Nitrofuran metatolites
Layering, thus fat is removed, while neutral alumina simultaneously also adsorbs fat, further improves clean-up effect,
Fat content is reduced, influence of the fat to testing result is reduced, and after centrifugation, neutral alumina is located at together with sample
Bottom solid phase, hexamethylene are located at top layer organic phase, are removed the upper and lower level of middle layer water phase A to fat simultaneously, have protected just rouge
The removal effect of fat avoids fat blocking solid-phase extraction column, so that making the speed of Solid Phase Extraction will not be blocked by fat and be subtracted
Slowly, fat is avoided to influence the ionization process of test substance.
It is purified using Solid Phase Extraction, realizes Nitrofuran metatolites and separated with the preferable of other impurities, together
When reduce the dosage of eluant, eluent, relative to directly mixing eluant, eluent with sample solution, carry out several times of liquid liquid extraction, reduce
The dosage of eluant, eluent, the eluent for blowing nitrogen are reduced, and are conducive to the reduction that nitrogen blows the time.
The present invention is further arranged to: in S1, with methanol: the volume ratio of water is 2:1, is cleaned to sample.
By using above-mentioned technical proposal, the free Nitrofuran metatolites outside sample are eliminated, are avoided outside sample
The free Nitrofuran metatolites that may be stained with impact last detection structure；Methanol makes protein denaturation, makes to dredge
The protein agglomeration of pine, thus it is more easily separated after protein centrifugation, advantageously reduce the appearance of miscellaneous peak.
The present invention is further arranged to: in S2, derivatization reagent is o-nitrobenzaldehyde.
The present invention is further arranged to: in S2, being carried out under light protected environment.
The present invention is further arranged to: in S3, promoting layering agent is sodium chloride solution.
By using above-mentioned technical proposal, sodium chloride solution increases the electrolyte strength of middle layer water phase A, makes middle layer water phase
The polarity gap of A and top layer organic phase becomes larger, to be conducive to accelerate the layered velocity of middle layer water phase A and top layer organic phase, makes
The Nitrofuran metatolites pretreatment process time is shorter.
The present invention is further arranged to: in S4, eluant, eluent is ethyl acetate.
The present invention is further arranged to: in S4, being taken middle layer water phase A to cross HLB pillar and is carried out Solid Phase Extraction.
The present invention is further arranged to: in S4, the specific steps of Solid Phase Extraction are as follows:
S1: successively using 3ml methanol, and 5ml water activates HLB pillar；
S2: crossing HLB pillar for middle layer water phase A with the speed of 1ml/min, elutes HLB pillar with 5ml water；
S3: HLB pillar is eluted with 5-10ml hexamethylene, efflux is discarded；
S4: and then HLB pillar is added with eluant, eluent and carries out affording eluent B.
By using above-mentioned technical proposal, after the activation of HLB pillar, after middle layer water phase A crosses HLB pillar, in the water phase of middle layer
Nitrofuran metatolites derivative adsorbed by HLB pillar, realize separation, then eluted with water, ensure that all middle layers
Water phase A all crosses HLB pillar, and water energy enough goes out the ionic species impurity in the water phase A of middle layer, ensure that in HLB pillar more
Completely, finally the water in HLB pillar is replaced out with hexamethylene, makes in the eluent B finally obtained with eluent
Water is less, and when nitrogen is blown, the boiling point of water is 100 DEG C, and boiling point is relatively high, is not easy to be blown out by nitrogen, and the boiling point of hexamethylene is
80.7 DEG C, the boiling point of acetonitrile is 81-82 DEG C, and the boiling point of ethyl acetate is 77 DEG C, to make the boiling point of hexamethylene and eluant, eluent
It is not much different, relative to water, is easier to be dried, advantageously reduces the time that eluent B is dried.
In conclusion advantageous effects of the invention are as follows:
1. accelerating the separating rate of Nitrofuran metatolites and protein, and be conducive to accelerate derivatization speed, make to derive
The time of change reduces, to be conducive to the reduction of Nitrofuran metatolites pretreatment process time；
2. the addition of hexamethylene, fat can incorporate in hexamethylene, and the water layer where hexamethylene and Nitrofuran metatolites point
Layer drops to fat be removed, while neutral alumina simultaneously also adsorbs fat, further improves clean-up effect
Low fat content reduces influence of the fat to testing result.
Specific embodiment
Embodiment 1
The pre-treating method of Nitrofuran metatolites, includes the following steps, the following are the preparations of testing sample solution:
S1: taking 2g sample (the present embodiment sample be pork sample), makes the methanol of 5mL volume ratio 2:1: aqueous solution to sample into
Row washing, cleans sample, blends sample and obtain sample, and 0.1 μ g/ml of 0.5ml, tetra- kinds of nitrofurans are added in the sample
Metabolin mixes internal standard standard solution (methanol dilution)；
S2: 10mL 0.2mol/L hydrochloric acid is added into sample and shakes even, the derivatization reagent (solvent of addition 0.3mL 0.05mol/L
For dimethyl sulfoxide), derivatization reagent is o-nitrobenzaldehyde, under light protected environment, ultrasound 1h at a temperature of 50 DEG C；
S3: with the sodium hydroxide solution tune PH to 7.4 of 1mol/L, the rush that 3ml 1mol/L is added is layered agent, and promoting layering agent is chlorine
Change sodium solution, be settled to 25ml with water, 10ml hexamethylene, 1g neutral alumina is added, it is solid to obtain bottom for refrigerated centrifuge after shaking
Phase, middle layer water phase A, top layer organic phase；
S4: successively using 3ml methanol, and 5ml water activates HLB pillar；
It takes the middle layer 10ml water phase A to cross HLB pillar with the speed of 1ml/min, elutes HLB pillar with 5ml water；
HLB pillar is eluted with 5ml hexamethylene, efflux is discarded；
Then it carries out 5ml eluant, eluent addition HLB pillar to afford eluent B, eluant, eluent is ethyl acetate, then with elution
Agent affords eluent B；
S5: eluent B is dried with nitrogen with 40 DEG C, and mobile phase is settled to 1mL when initial, 0.2 μm of filter membrane is crossed after mixing, with to be measured
It is fixed.
Embodiment 2
Difference from example 1 is that: in S2, ultrasound 1.2h at a temperature of 60 DEG C.
Embodiment 3
Difference from example 1 is that: in S2, ultrasound 1.5h at a temperature of 65 DEG C,
Embodiment 4
With embodiment 2 the difference is that: in S4, with 7ml hexamethylene elute HLB pillar.
Embodiment 5
With embodiment 2 the difference is that: in S4, with 10ml hexamethylene elute HLB pillar.
Comparative example 1: using the method in GB/T20752-2006.
Detection data:
It is used in conjunction using liquid chromatography-mass spectrography
1, instrument condition (identical as the instrument condition in GB/T20752-2006):
1.1 liquid phase chromatogram condition
Chromatographic column: Atlantis-C18 column (2.1 × 150mm, 3.5 μm)；
Mobile phase: as shown in table 1；
Flow velocity: 200 μ L/min；
Column temperature: 35 DEG C；
Sample volume: 40 μ L.
Table 1- eluent gradient elution requirement:
| Time (min) | 0.3% acetic acid aqueous solution (%) | 0.3% acetic acid acetonitrile solution (%) |
| 0.00 | 80 | 20 |
| 3.00 | 80 | 20 |
| 8.00 | 60 | 40 |
| 8.01 | 10 | 90 |
| 16.00 | 80 | 20 |
1.2 Mass Spectrometry Conditions
Ion source: ESI ion source；
Scanning mode: cation scanning；
Spray voltage: 5000V；
Assist gas (AUX) flow velocity: 7L/min；
It assists temperature degree (TEM): 480 DEG C；
Focus voltage (FP): 150V；
Collision cell exit potential (CXP)；11V；
Remove cluster voltage (DP): 45V；
The qualitative ion pair of four kinds of metabolites of nitrofuran and internal standard derivative, qualitative ion pair, acquisition time and collision gas energy
Mass spectrum is measured referring to table 2.
The mass spectrometry parameters of table 2- tetra- kinds of metabolites of nitrofuran and internal standard derivative:
2, measuring method is verified
2.1, the range of linearity and related coefficient
Under the experiment condition of embodiment 4, it is dense that four kinds of metabolites of nitrofuran mixed standard solutions are prepared with vehicle solution
Degree records chromatogram in 0.5,1,2,4,10ng/ml, sample introduction, draws standard curve, and calculate equation of linear regression, linear side
Journey and related coefficient are shown in Table 3.
Table 3- regression equation and related coefficient
As can be seen from Table 3, the related coefficient of this method is all larger than 0.99, is 0.5- in four kinds of metabolites of nitrofuran concentration
It is linear good within the scope of 10ng/ml；And the detection limit of 4 kinds of Nitrofuran metatolites is calculated with 3 times of signal-to-noise ratio (S/N)
(LOD) it is 0.2 μ g/kg, calculates the detection limit (LOD) of 4 kinds of Nitrofuran metatolites with 10 times of signal-to-noise ratio (S/N) as 0.5 μ g/
kg。
2.2, recovery test is added
Under the experimental condition of embodiment 4, in the bare substrate without determinand, after the cleaning of S1 step, addition
Four kinds of metabolites of nitrofuran mixed standard solutions of various concentration, the rate of recovery and average recovery rate are shown in Table 4.
2.3 Precision Experiment
Under conditions of 2.2, each the same terms one do 5 groups of parallel tests, and RSD value is shown in Table 4.
Table 4- metabolites of nitrofuran TIANZHU XINGNAO Capsul and relative standard deviation table (n=5)
As shown in Table 4, for each metabolin in the case where different metabolites of nitrofuran adds concentration, the rate of recovery is most of in 88-97%
In orientation, and RSD range, between 1.13-3.51%, so that the rate of recovery is good, precision is good.
3, under the conditions of embodiment 1-5 is respective and under conditions of comparative example 1, addition concentration is four kinds of 4 μ g/kg
Metabolites of nitrofuran mixed standard solution, the rate of recovery and nitrogen blow the time and are shown in Table 5.
The table 5- rate of recovery and nitrogen blow timetable
According to table 5 as can be seen that the rate of recovery of embodiment 1-5 is not much different with the rate of recovery in comparative example substantially, illustrate the party
Method reaches the rate of recovery of national regulations；The derivatization time of the derivatization time of 16h relative to comparative example 1, embodiment 1-5 exist
In the range of 1-1.5h, the derivatization time is greatly saved.
In embodiment 1-3, the rate of recovery of embodiment 1 is lower than embodiment 2 and 3, and the rate of recovery of embodiment 2 and 3 difference is not
Greatly, illustrate that the Extendible Extent of embodiment 2 and 3 is greater than embodiment 1, embodiment 2 is compared with 3, the elongating temperature of embodiment 3 and time
It lengthens, but the rate of recovery is not much different, and illustrates under conditions of embodiment 2, has been essentially derivative terminal, but embodiment 3
The derivatization time be greater than embodiment 2 the derivatization time, in order to further decrease the time of entire pre-treatment, optimal conditions is
Condition in embodiment 2.
For embodiment 2,4,5 compared with comparative example 1, nitrogen blows time reduction 30min or more, hence it is evident that reduces eluent B and is blown
The dry time, and 5ml-10ml hexamethylene by time of pillar in 4-8min, so that nitrogen is blown the time and shorten, so hexamethylene
The addition of alkane reduces nitrogen and blows the time；It is compared between embodiment 2,4,5, the nitrogen of embodiment 2 blows the time greater than embodiment 4 and 5, in fact
It applies in example 4 and 5, the increase of the hexamethylene of embodiment 5, the drying time change for blowing nitrogen is little, and embodiment 5 is than in embodiment 4
Hexamethylene amount it is more, in addition extra hexamethylene cross pillar needed for the time, the elution of embodiment 4 and 5 and nitrogen blow time base
This is close, but solvent needed for embodiment 4 is less, more saves, so optimal conditions is the condition in embodiment 4.
The embodiment of present embodiment is presently preferred embodiments of the present invention, not limits protection of the invention according to this
Range, therefore: the equivalence changes that all structures under this invention, shape, principle are done, should all be covered by protection scope of the present invention it
It is interior.
Claims (8)
1. the pre-treating method of Nitrofuran metatolites, it is characterised in that: the following steps are included:
S1: cleaning sample, blends sample and obtains sample；
S2: hydrochloric acid and derivatization reagent, the ultrasound 1-1.5h at a temperature of 50-65 DEG C are added into sample；
S3: adjusting PH to 7.4, and hexamethylene, neutral alumina is added and promotees layering agent, it is solid to obtain bottom for refrigerated centrifuge after shaking
Phase, middle layer water phase A, top layer organic phase；
S4: it takes middle layer water phase A to carry out Solid Phase Extraction, then obtains eluent B with eluent；
S5: eluent B is dried with nitrogen, mobile phase constant volume when initial.
2. the pre-treating method of Nitrofuran metatolites according to claim 1, it is characterised in that: in S1, use first
Alcohol: the volume ratio of water is 2:1, is cleaned to sample.
3. the pre-treating method of Nitrofuran metatolites according to claim 1, it is characterised in that: derivative in S2
Change reagent is o-nitrobenzaldehyde.
4. the pre-treating method of Nitrofuran metatolites according to claim 1, it is characterised in that: in S2, keeping away
It is carried out under luminous environment.
5. the pre-treating method of Nitrofuran metatolites according to claim 1, it is characterised in that: in S3, promote to divide
Layer agent is sodium chloride solution.
6. the pre-treating method of Nitrofuran metatolites according to claim 1, it is characterised in that: in S4, elution
Agent is ethyl acetate.
7. the pre-treating method of Nitrofuran metatolites according to claim 1, it is characterised in that: in S4, take
Layer water phase A crosses HLB pillar and carries out Solid Phase Extraction.
8. the pre-treating method of Nitrofuran metatolites according to claim 1, it is characterised in that: in S4, solid phase
The specific steps of extraction are as follows:
S1: successively using 3ml methanol, and 5ml water activates HLB pillar；
S2: crossing HLB pillar for middle layer water phase A with the speed of 1ml/min, elutes HLB pillar with 5ml water；
S3: HLB pillar is eluted with 5-10ml hexamethylene, efflux is discarded；
S4: and then HLB pillar is added with eluant, eluent and carries out affording eluent B.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110836938A (en) * | 2019-12-05 | 2020-02-25 | 广州智汇生物科技有限公司 | Detection method of furan metabolites in aquatic products and preparation method of solid-phase extraction column |
| CN111207991A (en) * | 2020-02-26 | 2020-05-29 | 杭州南开日新生物技术有限公司 | Pretreatment method and detection method of nitrofuran metabolite |
| CN114487171A (en) * | 2022-01-06 | 2022-05-13 | 唐山市食品药品综合检验检测中心(唐山市农产品质量安全检验检测中心、唐山市检验检测研究院) | Detection method and application of nitrofuran metabolites in aquatic products |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103091418A (en) * | 2013-01-15 | 2013-05-08 | 新希望乳业控股有限公司 | Method for detecting plasticizing agent |
| CN104297384A (en) * | 2014-09-05 | 2015-01-21 | 北京华都肉鸡公司 | Detection method of nitrofuran drug metabolites in meat product |
| CN104374910A (en) * | 2014-11-19 | 2015-02-25 | 无锡中德伯尔生物技术有限公司 | Kit and method applied to detection of nitrofurans drug metabolite |
| CN106124653A (en) * | 2016-06-16 | 2016-11-16 | 中国水产科学研究院黄海水产研究所 | 5 kinds of Nitrofuran metatolites and the detection method of the many residuals of chloromycetin in shrimp |
| CN107607643A (en) * | 2017-09-08 | 2018-01-19 | 长乐聚泉食品有限公司 | The detection method of Nitrofuran metabolites in eel |
| CN108008038A (en) * | 2017-11-26 | 2018-05-08 | 杭州市食品药品检验研究院 | Measure four kinds of remaining methods of Nitrofuran metabolites metabolite in gelatin type traditional Chinese medicine |
| CN108845063A (en) * | 2018-06-21 | 2018-11-20 | 中国中医科学院中药研究所 | The test reagent combination and detection method of aquatic products additive |
| CN109580890A (en) * | 2019-01-24 | 2019-04-05 | 梧州市食品药品检验所 | The measuring method of Nitrofuran metabolites in a kind of pork |
| CN109632427A (en) * | 2019-01-28 | 2019-04-16 | 广州食源生物科技有限公司 | A kind of pre-treating method that Nitrofuran metatolites quickly detect and its detection method |
-
2019
- 2019-08-13 CN CN201910745489.8A patent/CN110361490A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103091418A (en) * | 2013-01-15 | 2013-05-08 | 新希望乳业控股有限公司 | Method for detecting plasticizing agent |
| CN104297384A (en) * | 2014-09-05 | 2015-01-21 | 北京华都肉鸡公司 | Detection method of nitrofuran drug metabolites in meat product |
| CN104374910A (en) * | 2014-11-19 | 2015-02-25 | 无锡中德伯尔生物技术有限公司 | Kit and method applied to detection of nitrofurans drug metabolite |
| CN106124653A (en) * | 2016-06-16 | 2016-11-16 | 中国水产科学研究院黄海水产研究所 | 5 kinds of Nitrofuran metatolites and the detection method of the many residuals of chloromycetin in shrimp |
| CN107607643A (en) * | 2017-09-08 | 2018-01-19 | 长乐聚泉食品有限公司 | The detection method of Nitrofuran metabolites in eel |
| CN108008038A (en) * | 2017-11-26 | 2018-05-08 | 杭州市食品药品检验研究院 | Measure four kinds of remaining methods of Nitrofuran metabolites metabolite in gelatin type traditional Chinese medicine |
| CN108845063A (en) * | 2018-06-21 | 2018-11-20 | 中国中医科学院中药研究所 | The test reagent combination and detection method of aquatic products additive |
| CN109580890A (en) * | 2019-01-24 | 2019-04-05 | 梧州市食品药品检验所 | The measuring method of Nitrofuran metabolites in a kind of pork |
| CN109632427A (en) * | 2019-01-28 | 2019-04-16 | 广州食源生物科技有限公司 | A kind of pre-treating method that Nitrofuran metatolites quickly detect and its detection method |
Non-Patent Citations (10)
| Title |
|---|
| 冯磊 等: "二次通用旋转组合设计法优化酶法提取茶叶籽蛋白工艺", 《食品工业科技》 * |
| 张宏宇: "基于氢键的聚合物多层膜的构筑与结构调控", 《中国优秀博硕士学位论文全文数据库（博士） 工程科技I辑》 * |
| 李兰杰 等: "超声辅助结合离子液体双水相提取-高效液相色谱法测定三七中5 种稀有人参皂苷的含量", 《高等学校化学学报》 * |
| 杨方: "复杂食品基体中痕量残留分离分析技术研究", 《中国优秀博硕士学位论文全文数据库（博士） 工程科技I辑》 * |
| 梁炜薇 等: "人参内生球毛壳菌株ＲSQMK-9 的化学成分研究", 《天然产物研究与开发》 * |
| 洪萍 等: "富马酸二甲酯检测方法的研究进展", 《中国卫生检验杂志》 * |
| 郑香平 等: "超高效液相色谱－串联质谱法测定水产品中孔雀石绿、结晶紫及其代谢物残留量", 《理化检验-化学分册》 * |
| 顾华兵 等: "鸡肉组织中氯丙嗪残留的HPLC-MS/MS检测方法的建立", 《中国家禽》 * |
| 高洁 等: "超高效液相色谱-串联质谱法测定多脂肪类动物源性食品中硝基呋喃代谢物", 《食品安全质量检测学报》 * |
| 黄瓒 等: "高效液相色谱法测定皮革中富马酸二甲酯", 《皮革科学与工程》 * |
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| CN110836938A (en) * | 2019-12-05 | 2020-02-25 | 广州智汇生物科技有限公司 | Detection method of furan metabolites in aquatic products and preparation method of solid-phase extraction column |
| CN111207991A (en) * | 2020-02-26 | 2020-05-29 | 杭州南开日新生物技术有限公司 | Pretreatment method and detection method of nitrofuran metabolite |
| CN114487171A (en) * | 2022-01-06 | 2022-05-13 | 唐山市食品药品综合检验检测中心(唐山市农产品质量安全检验检测中心、唐山市检验检测研究院) | Detection method and application of nitrofuran metabolites in aquatic products |
| CN114487171B (en) * | 2022-01-06 | 2022-09-16 | 唐山市食品药品综合检验检测中心(唐山市农产品质量安全检验检测中心、唐山市检验检测研究院) | Detection method and application of nitrofuran metabolites in aquatic products |
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