CN104931610A - Method for simultaneously measuring 16 sulfonamides in beewax by high performance liquid chromatography tandem mass spectrometry - Google Patents
Method for simultaneously measuring 16 sulfonamides in beewax by high performance liquid chromatography tandem mass spectrometry Download PDFInfo
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Abstract
The invention relates to an inspection and quarantine method, and particularly relates to a method for simultaneously measuring 16 sulfonamides in beewax by high performance liquid chromatography tandem mass spectrometry. According to the method provided by the invention, normal hexane is adopted for pre-dissolution, a formic acid aqueous solution is extracted, an MCX solid phase extraction column is used for purification, an Agilent Eclipse Plus-18 column (100mm times 2.1mm, 3.5 microns) is used for separating, and an electrospray ion source positive ion multi-reaction monitor (MRM) mode tandem mass spectrum is used for measuring. The 16 sulfonamides, provided by the invention, respectively have better linear relation in a range of 2ng/mL to 50 ng/mL, and the correlation coefficients are larger than 0.995. Under the adding levels of 2.0 mu. g/kg, 5.0 mu. g/kg and 10.0 mu. g/kg, the recovery rate of the 16 sulfonamides in a practical sample is 65 to 127 percent, the relative standard deviation is (RSD, n is equal to 6) is 2.9 to 13.5 percent, and the limit of quantitation (S/N is more than 10) is 2.0 mu. g/kg. The method is quick, sensitive, accurate, and suitable for qualitative analysis and quantitative analysis of the residual of the 16 sulfonamides in a daily beewax sample.
Description
Technical field
The present invention relates to a kind of inspection and quarantine method, particularly relate to the method for 16 kinds of sulfa drugss in a kind of using high performance liquid chromatography tandem mass spectrum method Simultaneously test beeswax.
Background technology
Sulfa drugs is the general name of a class extensive pedigree antibiotic with P-aminobenzene-sulfonamide structure, because it has has a broad antifungal spectrum, efficient, low toxicity, lower-price characteristic, is widely used in prevention and therapy bacterial infection disease in livestock breeding industry.Because this medicine metabolism time is in vivo longer, will produce infringement to the function of human body when reaching finite concentration, destroy the hemopoietic system of people, affecting health, also there is potential carcinogenicity in sulfamethazine etc.At present, detect sulfa drugs in the animal derived food such as bee product, aquatic products and generally adopt liquid chromatography-fluorescence detector method and liquid phase chromatogram-mass spectrometry combination method.
Beeswax is a kind of material secreted by the four pairs of wax glands below worker bee belly, and its principal ingredient is the ester class etc. that alkanol and alkanoic acid are formed, cosmetics, food and medicine industrial have apply more widely.Matrix due to beeswax is different from honey, royal jelly, and it cannot adopt sulfonamides object detecting method in existing honey, royal jelly to detect.For ensureing the Safety of Food Quality of current beeswax, prevent sulfa drugs by bee products such as beeswax indirect pollution honey, royal jelly.Be badly in need of the method setting up sulfa drugs in a kind of using high performance liquid chromatography tandem mass spectrum method Simultaneously test beeswax.
Summary of the invention
In order to solve above-mentioned technical matters, the object of this invention is to provide the method for sulfa drugs in a kind of using high performance liquid chromatography tandem mass spectrum method Simultaneously test beeswax, the advantages such as this method is easy, highly sensitive, matrix interference is little, may be used for the qualitative and quantitative analysis of sulfa drug residue in beeswax sample.
In order to realize above-mentioned object, present invention employs following technical scheme:
The method of 16 kinds of sulfa drugss in using high performance liquid chromatography tandem mass spectrum method Simultaneously test beeswax; 16 kinds of described sulfa drugss are sulfameter, cistosulfa, sulfadimethoxine, sulfbenzamide, sulfamethyldiazine, sulfamethazine, sulfanilamide (SN) Sulfafurazole, sulfamonomethoxine, Sulfaquinoxaline, sulphadiazine, sulphathiazole, sulfamethoxypyridazine, ayerlucil, sulfamethoxazole, sulfapryidine and fanasil, and the method comprises the following steps:
1) instrument and reagent are selected
1.1) instrument
1260 Ultra Performance Liquid Chromatography-6460 triple quadrupole bar tandem mass spectrum combined instruments, Agilent company of the U.S.; MS 3 digital eddy mixer, German IKA company; N-EVAP-111 Nitrogen evaporator, Organomation company of the U.S.; Multifuge X1R hydro-extractor, Thermo Scientific company of the U.S.;
1.2) reagent:
Standard items: sulfameter, cistosulfa, sulfadimethoxine, sulfbenzamide, sulfamethyldiazine, sulfamethazine, sulfanilamide (SN) Sulfafurazole, sulfamonomethoxine, Sulfaquinoxaline, sulphadiazine, sulphathiazole, sulfamethoxypyridazine, ayerlucil, sulfamethoxazole, sulfapryidine and fanasil; Methyl alcohol, normal hexane, formic acid are chromatographically pure; Ammoniacal liquor: 25%-28%; MCX solid phase extraction column: 500mg/6mL Town in Shanghai spectrum company;
2) standard working solution
2.1) standard reserving solution
Accurately take 0.025g16 kind sulfa drugs standard items respectively in beaker, dissolve with methyl alcohol, lysate is all transferred in 25mL volumetric flask uses methanol rinses 3 times respectively, rinse liquid is all transferred in volumetric flask, by methanol constant volume to scale, be mixed with the standard reserving solution that concentration is 1mg/mL, labelled;
2.2) the hybrid standard storing solution of 100 μ g/mL
Accurately draw above-mentioned 16 kinds of standard reserving solutions of 1mL respectively in 10mL volumetric flask, with methanol dilution to scale, be mixed with the hybrid standard storing solution that concentration is 100 μ g/mL;
2.3) the hybrid standard storing solution of 10ug/mL
The above-mentioned 16 kinds of hybrid standard storing solutions of accurate absorption 1mL, in 10mL volumetric flask, with methanol dilution to scale, are mixed with the hybrid standard storing solution that concentration is 10ug/mL;
2.4) the hybrid standard storing solution of 1ug/mL
Accurate absorption 1mL hybrid standard storing solution, in 10mL volumetric flask, with methanol dilution to scale, is mixed with the hybrid standard storing solution that concentration is 1ug/mL;
2.5) mark mixed solution in
Accurately take a certain amount of sulfapryidine-D4, sulfamethazine-D4, sulfamethoxazole-D4, sulfaquinoxaline, 13C6, sulphadiazine-D4, sulphathiazole-D4, be mixed with the interior mark mixed solution that concentration is 200ng/mL;
2.6) hybrid standard working fluid
Accurately pipette a certain amount of above-mentioned hybrid standard storing solution and interior mark mixed solution respectively, be mixed with pure water dilution the standard working solution that concentration is respectively 5ng/mL, 10ng/mL, 20ng/mL, 40ng/mL, 50ng/mL;
3) extract
Take sample 2g, be accurate to 0.01g, be placed in 50mL tool plug plastic centrifuge tube, add the mixing interior mark 50uL that concentration is 200ng/mL, add 10mL normal hexane, adding 10mL concentration of volume percent after vortex ultrasonic dissolution is that 1% aqueous formic acid vortex oscillation is extracted, the centrifugal 5min of 8000r/min, get lower aqueous layer, to be clean;
4) purify
Be transferred to by extract in MCX solid phase extraction column, MCX solid phase extraction column is use 5mL methyl alcohol successively before 500mg/6mL, MCX solid phase extraction column uses, and 5mL concentration of volume percent is the aqueous formic acid activation of 1%; Discard leacheate, with the drip washing of 5.0mL methanol-water solution, methanol-water solution volume ratio is 1:1, drains, by 8mL 5% ammoniacal liquor methanol-eluted fractions, collect whole eluent, below 50 DEG C, in water-bath, nitrogen dries up, and dissolve with 2.0mL methyl alcohol-0.15% formic acid solution, methyl alcohol-0.15% formic acid solution volume ratio is that 1:9 shakes up, after sample liquid crosses 0.45um membrane filtration, measure for liquid chromatography-tandem mass spectrometry;
5) chromatographic condition
Chromatographic column: Agilent Eclipse Plus-C18 post, 100 × 2.1mm, 3.5 μm; Column temperature: 40 DEG C; Sample size: 20 μ L; Mobile phase: A is concentration of volume percent is 0.15% aqueous formic acid, and B is acetonitrile, and condition of gradient elution is as follows:
6) Mass Spectrometry Conditions
Scan mode: holotype scans; Detection mode: multiple-reaction monitoring (MRM); Dry gas temperature (Gas Temp): 325 DEG C; Dry gas flow (Gas Flow): 5L/min; Spray pressure power (Nebulizer): 45psi; Sheath temperature degree (Sheath GasTemp): 400 DEG C; Sheath gas velocity (Sheath Gas Flow): 12L/min; Capillary voltage (Capillary): 4000V; The Mass Spectrometry Conditions of 16 kinds of sulfa drugss is as follows:
* quota ion.
The present invention, owing to have employed above-mentioned technical scheme, establishes the Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry Analysis method of 16 kinds of sulfa drugss (sulfameter, cistosulfa, sulfadimethoxine, sulfbenzamide, sulfamethyldiazine, sulfamethazine, sulfanilamide (SN) Sulfafurazole, sulfamonomethoxine, Sulfaquinoxaline, sulphadiazine, sulphathiazole, sulfamethoxypyridazine, ayerlucil, sulfamethoxazole, sulfapryidine, fanasil) in Simultaneously test beeswax.Sample adopts normal hexane predissolve, aqueous formic acid extracts, purify through MCX solid phase extraction column, with AgilentEclipse Plus-C18 post (100mm × 2.1mm, 3.5 μm) be separated, electric spray ion source positive ion multiple-reaction monitoring (MRM) pattern tandem mass spectrum measures.Investigate and optimize extraction, purification method and Instrument measuring condition etc. herein.Result shows, 16 kinds of sulfa drugss all have good linear relationship within the scope of 2ng/mL-50ng/mL, and related coefficient is greater than 0.995.Under 2.0 μ g/kg, 5.0 μ g/kg and 10.0 μ g/kg Pitch-based sphere, in actual sample, the recovery of 16 kinds of sulfa drugss is between 65%-127%, relative standard deviation (RSD, n=6) between 2.9%-13.5%, method quantitative limit (S/N>10) is 2.0 μ g/kg.This method is quick, sensitive, accurate, is applicable to the qualitative and quantitative analysis of 16 kinds of sulfa drug residues in daily beeswax sample.
Accompanying drawing explanation
The total ion current figure (Pitch-based sphere 2.0 μ g/kg) of 16 kinds of sulfanilamide (SN) in Fig. 1 beeswax.
The total ion current figure (Pitch-based sphere 5.0 μ g/kg) of 16 kinds of sulfanilamide (SN) in Fig. 2 beeswax.
The total ion current figure (Pitch-based sphere 10.0 μ g/kg) of 16 kinds of sulfanilamide (SN) in Fig. 3 beeswax.
The MRM chromatogram (Pitch-based sphere 2.0 μ g/kg) of sulphadiazine in Fig. 4 beeswax.
The MRM chromatogram (Pitch-based sphere 2.0 μ g/kg) of sulphathiazole in Fig. 5 beeswax.
The MRM chromatogram (Pitch-based sphere 2.0 μ g/kg) of sulfapryidine in Fig. 6 beeswax.
The MRM chromatogram (Pitch-based sphere 2.0 μ g/kg) of sulfamethyldiazine in Fig. 7 beeswax.
The MRM chromatogram (Pitch-based sphere 2.0 μ g/kg) of sulfamethazine in Fig. 8 beeswax.
The MRM chromatogram (Pitch-based sphere 2.0 μ g/kg) of sulfamethoxypyridazine in Fig. 9 beeswax.
The MRM chromatogram (Pitch-based sphere 2.0 μ g/kg) of sulfbenzamide in Figure 10 beeswax.
The MRM chromatogram (Pitch-based sphere 2.0 μ g/kg) of sulfanilamide (SN) sulfameter in Figure 11 beeswax.
The MRM chromatogram (Pitch-based sphere 2.0 μ g/kg) of sulfamonomethoxine in Figure 12 beeswax.
The MRM chromatogram (Pitch-based sphere 2.0 μ g/kg) of Sulfaquinoxaline in Figure 13 beeswax.
The MRM chromatogram (Pitch-based sphere 2.0 μ g/kg) of fanasil in Figure 14 beeswax.
The MRM chromatogram (Pitch-based sphere 2.0 μ g/kg) of sulfadimethoxine in Figure 15 beeswax.
The MRM chromatogram (Pitch-based sphere 2.0 μ g/kg) of sulfamethoxazole in Figure 16 beeswax.
The MRM chromatogram (Pitch-based sphere 2.0 μ g/kg) of ayerlucil in Figure 17 beeswax.
The MRM chromatogram (Pitch-based sphere 2.0 μ g/kg) of cistosulfa in Figure 18 beeswax.
The MRM chromatogram (Pitch-based sphere 2.0 μ g/kg) of sulfanilamide (SN) Sulfafurazole in Figure 19 beeswax.
Embodiment
1 experimental section
1.1 instruments and reagent
1260 Ultra Performance Liquid Chromatography-6460 triple quadrupole bar tandem mass spectrums combined instrument (Agilent company of the U.S.); MS 3 digital eddy mixer (German IKA company); N-EVAP-111 Nitrogen evaporator (Organomation company of the U.S.); Multifuge X1R hydro-extractor (Thermo Scientific company of the U.S.).
Standard items (German Dr company); Methyl alcohol, normal hexane, formic acid are chromatographically pure, ammoniacal liquor: 25%-28%; MCX solid phase extraction column: 500mg/6mL (Town in Shanghai spectrum company).
1.2 standard working solution
1.2.1 standard reserving solution (1mg/mL)
Accurately take 0.025g standard items (sulfameter respectively, cistosulfa, sulfadimethoxine, sulfbenzamide, sulfamethyldiazine, sulfamethazine, sulfanilamide (SN) Sulfafurazole, sulfamonomethoxine, Sulfaquinoxaline, sulphadiazine, sulphathiazole, sulfamethoxypyridazine, ayerlucil, sulfamethoxazole, sulfapryidine, fanasil) in beaker, dissolve with methyl alcohol, lysate is all transferred in 25mL volumetric flask uses methanol rinses 3 times respectively, rinse liquid is all transferred in volumetric flask, by methanol constant volume to scale, be mixed with the standard reserving solution that concentration is 1mg/mL, labelled.
1.2.2 hybrid standard storing solution (100 μ g/mL)
Accurately draw above-mentioned 16 kinds of standard reserving solutions (1mg/mL) of 1mL respectively in 10mL volumetric flask, with methanol dilution to scale, be mixed with the hybrid standard storing solution that concentration is 100 μ g/mL.
1.2.3 hybrid standard storing solution (10ug/mL)
The above-mentioned 16 kinds of hybrid standard storing solutions of accurate absorption 1mL (100 μ g/mL), in 10mL volumetric flask, with methanol dilution to scale, are mixed with the hybrid standard storing solution that concentration is 10ug/mL.
1.2.4 hybrid standard storing solution (1ug/mL)
Accurate absorption 1mL hybrid standard storing solution (10ug/mL), in 10mL volumetric flask, with methanol dilution to scale, is mixed with the hybrid standard storing solution that concentration is 1ug/mL.
1.2.5 mark standard solution (100ng/mL) in mixing
Accurately take a certain amount of sulfapryidine-D4, sulfamethazine-D4, sulfamethoxazole-D4, sulfaquinoxaline, 13C6, sulphadiazine-D4, sulphathiazole-D4, be mixed with the interior mark mixed solution that concentration is 200ng/mL.
1.2.6 hybrid standard working fluid
Accurately pipette a certain amount of above-mentioned hybrid standard storing solution and mixing inner mark solution respectively, be mixed with pure water dilution the standard working solution that concentration is respectively 5ng/mL, 10ng/mL, 20ng/mL, 40ng/mL, 50ng/mL.
1.3 extract
Take sample 2g (being accurate to 0.01g), be placed in 50mL tool plug plastic centrifuge tube, add the mixing interior mark 50uL that concentration is 200ng/mL, add 10mL normal hexane, add 10mL aqueous formic acid (1%) vortex oscillation after vortex ultrasonic dissolution to extract, the centrifugal 5min of 8000r/min, gets lower aqueous layer, to be clean.
1.4 purification
Extract is transferred to MCX solid phase extraction column (500mg/6mL, 5mL methyl alcohol is used successively before using, 5mL aqueous formic acid (1%) activates) in, discard leacheate, with 5.0mL methanol-water (1:1, V/V) drip washing, drain, by 8mL 5% ammoniacal liquor methanol-eluted fractions, collect whole eluent, below 50 DEG C, in water-bath, nitrogen dries up, with 1.0mL methyl alcohol-0.15% formic acid (1:9) solubilize, shake up, after sample liquid crosses 0.45um membrane filtration, measure for liquid chromatography-tandem mass spectrometry.
1.5 chromatographic condition
Chromatographic column: Agilent Eclipse Plus-C18 post (100 × 2.1mm, 3.5 μm); Column temperature: 40 DEG C; Sample size: 20 μ L.Mobile phase: A is 0.15% aqueous formic acid, and B is acetonitrile, and condition of gradient elution is in table 1.
Table 1 condition of gradient elution
1.6 Mass Spectrometry Conditions
Scan mode: holotype scans; Detection mode: multiple-reaction monitoring (MRM); Dry gas temperature (Gas Temp): 325 DEG C; Dry gas flow (Gas Flow): 5L/min; Spray pressure power (Nebulizer): 45psi; Sheath temperature degree (Sheath GasTemp): 400 DEG C; Sheath gas velocity (Sheath Gas Flow): 12L/min; Capillary voltage (Capillary): 4000V.
The Mass Spectrometry Conditions of table 2 sulfa drugs
* quota ion
2 results and discussion
2.1 Extraction solvent are selected
The principal ingredient of beeswax has free fatty acid, free alkyl alcohol, carbohydrates, carotenoid etc., belongs to liposoluble substance
[1].So after employing adds n-hexane dissolution beeswax sample, then add sulfa drugs in aqueous formic acid extraction beeswax sample herein.Shown by recovery test, the method effectively can extract the mensuration material in beeswax.
The range of linearity of 2.2 methods and detection limit
Prepare a series of variable concentrations standard working solution (2.0,5.0,10,20,40,50ng/mL), and sample introduction successively, respectively to measure the peak area Y of object for ordinate, with corresponding concentration value for horizontal ordinate, make typical curve, in table 2, result shows, 16 kinds of sulfamido objects its concentration and peak area within the scope of 2 ~ 50ng/mL are good linear relationship, coefficient R
2be greater than 0.994.
In negative sample, add target compound, measure according to method herein, the Pitch-based sphere of 10 times of signal to noise ratio (S/N ratio) (S/N) correspondences, as quantitative limit (LOQ), the results are shown in Table 3.
Table 316 kind of sulfa drugs linear equation, detection limit, quantitative limit (unit: μ g/kg)
The recovery of 2.4 methods and precision
The method of carrying out adding in negative sample standard solution under 2.0 μ g/kg, 5.0 μ g/kg and 10.0 μ g/kg, tri-Pitch-based sphere carries out method recovery test, and each Pitch-based sphere repeats 6 times, and the method recovery and precision are in table 4.Result shows, the recovery of standard addition scope of 16 kinds of sulfa drugss is between 65%-127%, and relative standard deviation (RSD) is 2.9%-13.5%, shows that the method developed can meet the requirement of routine testing herein.
The TIANZHU XINGNAO Capsul of target analytes and precision (n=6) in table 4 negative sample
3 conclusions
This experiment adopts normal hexane predissolve, and acidic aqueous solution extracts, the pre-treating method extraction and cleanings such as MCX solid phase extraction column purification, and Ultra Performance Liquid Chromatography-tandem mass spectrum Internal standard measures 16 kinds of sulfa drugss in beeswax.Result shows, this method has easy, sensitive, advantage accurately, may be used for the qualitative and quantitative analysis of trace sulfa drug residue in beeswax.
Claims (1)
1. the method for 16 kinds of sulfa drugss in using high performance liquid chromatography tandem mass spectrum method Simultaneously test beeswax; it is characterized in that 16 kinds of described sulfa drugss are sulfameter, cistosulfa, sulfadimethoxine, sulfbenzamide, sulfamethyldiazine, sulfamethazine, sulfanilamide (SN) Sulfafurazole, sulfamonomethoxine, Sulfaquinoxaline, sulphadiazine, sulphathiazole, sulfamethoxypyridazine, ayerlucil, sulfamethoxazole, sulfapryidine and fanasil, the method comprises the following steps:
1) instrument and reagent are selected
1.1) instrument
1260 Ultra Performance Liquid Chromatography-6460 triple quadrupole bar tandem mass spectrum combined instruments, Agilent company of the U.S.; MS 3 digital eddy mixer, German IKA company; N-EVAP-111 Nitrogen evaporator, Organomation company of the U.S.; Multifuge X1R hydro-extractor, Thermo Scientific company of the U.S.;
1.2) reagent:
Standard items: sulfameter, cistosulfa, sulfadimethoxine, sulfbenzamide, sulfamethyldiazine, sulfamethazine, sulfanilamide (SN) Sulfafurazole, sulfamonomethoxine, Sulfaquinoxaline, sulphadiazine, sulphathiazole, sulfamethoxypyridazine, ayerlucil, sulfamethoxazole, sulfapryidine and fanasil; Methyl alcohol, normal hexane, formic acid are chromatographically pure; Ammoniacal liquor: 25%-28%; MCX solid phase extraction column: 500mg/6mL Town in Shanghai spectrum company;
2) standard working solution
2.1) standard reserving solution
Accurately take 0.025g16 kind sulfa drugs standard items respectively in beaker, dissolve with methyl alcohol, lysate is all transferred in 25mL volumetric flask uses methanol rinses 3 times respectively, rinse liquid is all transferred in volumetric flask, by methanol constant volume to scale, be mixed with the standard reserving solution that concentration is 1mg/mL, labelled;
2.2) the hybrid standard storing solution of 100 μ g/mL
Accurately draw in above-mentioned 16 kinds of standard reserving solution to 10 mL volumetric flasks of 1 mL respectively, with methanol dilution to scale, be mixed with the hybrid standard storing solution that concentration is 100 μ g/mL;
2.3) the hybrid standard storing solution of 10ug/mL
In above-mentioned 16 kinds of hybrid standard storing solution to the 10 mL volumetric flasks of accurate absorption 1 mL, with methanol dilution to scale, be mixed with the hybrid standard storing solution that concentration is 10ug/mL;
2.4) the hybrid standard storing solution of 1ug/mL
In accurate absorption 1 mL hybrid standard storing solution to 10 mL volumetric flask, with methanol dilution to scale, be mixed with the hybrid standard storing solution that concentration is 1ug/mL;
2.5) mark mixed solution in
Accurately take a certain amount of sulfapryidine-D4, sulfamethazine-D4, sulfamethoxazole-D4, sulfaquinoxaline, 13C6, sulphadiazine-D4, sulphathiazole-D4, be mixed with the interior mark mixed solution that concentration is 200ng/mL;
2.6) hybrid standard working fluid
Accurately pipette a certain amount of above-mentioned hybrid standard storing solution and interior mark mixed solution respectively, be mixed with pure water dilution the standard working solution that concentration is respectively 5ng/mL, 10ng/mL, 20ng/mL, 40 ng/mL, 50ng/mL;
3) extract
Take sample 2 g, be accurate to 0.01g, be placed in 50 mL tool plug plastic centrifuge tubes, add the interior mark of mixing 50 uL that concentration is 200 ng/mL, add 10 mL normal hexanes, adding 10 mL concentration of volume percent after vortex ultrasonic dissolution is that 1% aqueous formic acid vortex oscillation is extracted, centrifugal 5 min of 8000 r/min, get lower aqueous layer, to be clean;
4) purify
Be transferred to by extract in MCX solid phase extraction column, MCX solid phase extraction column is use 5 mL methyl alcohol successively before 500mg/6mL, MCX solid phase extraction column uses, and 5 mL concentration of volume percent are the aqueous formic acid activation of 1%; Discard leacheate, with 5.0 mL methanol-water solution drip washing, methanol-water solution volume ratio is 1:1, drains, by 8mL 5% ammoniacal liquor methanol-eluted fractions, collect whole eluent, below 50 DEG C, in water-bath, nitrogen dries up, and dissolve with 2.0mL methyl alcohol-0.15% formic acid solution, methyl alcohol-0.15% formic acid solution volume ratio is that 1:9 shakes up, after sample liquid crosses 0.45um membrane filtration, measure for liquid chromatography-tandem mass spectrometry;
5) chromatographic condition
Chromatographic column: Agilent Eclipse Plus-C18 post, 100 × 2.1 mm, 3.5 μm; Column temperature: 40 DEG C; Sample size: 20 μ L; Mobile phase: A is concentration of volume percent is 0.15% aqueous formic acid, and B is acetonitrile, and condition of gradient elution is as follows:
6) Mass Spectrometry Conditions
Scan mode: holotype scans; Detection mode: multiple-reaction monitoring (MRM); Dry gas temperature (Gas Temp): 325 DEG C; Dry gas flow (Gas Flow): 5 L/min; Spray pressure power (Nebulizer): 45 psi; Sheath temperature degree (Sheath Gas Temp): 400 DEG C; Sheath gas velocity (Sheath Gas Flow): 12 L/min; Capillary voltage (Capillary): 4000 V; The Mass Spectrometry Conditions of 16 kinds of sulfa drugss is as follows:
* quota ion.
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| CN108931599B (en) * | 2018-05-25 | 2021-06-01 | 无锡微色谱生物科技有限公司 | Method for extracting and analyzing sulfonamides by using DPX gun head type dispersed solid phase microextraction column |
| CN109738538A (en) * | 2019-01-18 | 2019-05-10 | 中国农业科学院蜜蜂研究所 | A method of identifying the mature honey of natural capping and honey is concentrated in hot-working |
| CN111650298A (en) * | 2020-06-09 | 2020-09-11 | 武汉市农业科学院 | Method for simultaneously detecting 5 sulfonamides in cow dung by solid-phase extraction-high performance liquid chromatography |
| CN114942289A (en) * | 2022-06-02 | 2022-08-26 | 贵州大学 | Method for determining anticoccidial drugs in water in surrounding environment of farm by liquid chromatography-mass spectrometry |
| CN114942289B (en) * | 2022-06-02 | 2023-05-16 | 贵州大学 | Method for measuring anticoccidial drug in water in surrounding environment of farm by liquid chromatography mass spectrometry |
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