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Determination of multi-veterinary drugs residues in pork, shrimp and honey for export. LC-MS/MS method
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Basic data
| Standard ID | SN/T 3155-2012 (SN/T3155-2012) |
| Description (Translated English) | Determination of multi-veterinary drugs residues in pork, shrimp and honey for export. LC-MS/MS method |
| Sector / Industry | Commodity Inspection Standard (Recommended) |
| Classification of Chinese Standard | X04 |
| Classification of International Standard | 67.050 |
| Word Count Estimation | 53,514 |
| Quoted Standard | GB/T 6682 |
| Regulation (derived from) | National Quality Inspection (2012) 237; |
| Issuing agency(ies) | General Administration of Customs |
| Summary | This standard specifies the pork, shrimp, many types of drug residues in honey determination of sample preparation and liquid chromatography mass spectrometry/mass spectrometry. This standard applies to pork, shrimp, honey sulfadiazine, sulfathiazole, sul |
SN/T 3155-2012: Determination of multi-veterinary drugs residues in pork, shrimp and honey for export. LC-MS/MS method
---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
Determination of multi-veterinary drugs residues in pork, shrimp and honey for export.LC-MS/MS method
People's Republic of China Entry-Exit Inspection and Quarantine Standards
Export pork, shrimp, honey and more drug residues
Determination of liquid chromatography - mass spectrometry/mass spectrometry
Issued on. 2012-05-07
2012-11-16 implementation
People's Republic of China
The State Administration of Quality Supervision, Inspection and Quarantine released
Foreword
This standard was drafted in accordance with GB/T 1.1-2009 given rules.
Please note that some of the content of this document may involve patents. Distribution of this document
Institutions do not assume the responsibility to identify these patents.
This standard is proposed and managed by the National Certification and Accreditation Administration Committee.
This standard was drafted. People's Republic of China Zhejiang Exit Inspection and Quarantine.
The main drafters of this standard. Chen Xiaomei Xie Wen, Hou Jianbo, Xijun Yang, Qian Yan, Wang Feng, Han Chao.
Export pork, shrimp, honey and more drug residues
Determination of liquid chromatography - mass spectrometry/mass spectrometry
1 Scope
This standard specifies the pork, shrimp and many types of drug residues in honey Determination of sample preparation and liquid chromatography - mass spectrometry/mass spectrometry.
This standard applies to pork, shrimp and honey sulfadiazine, Sulfathiazole, sulfasalazine, sulfamethyldiazine, sulfamethazine, sulfonamide
Amine-5- (p) pyrimidine methicillin, sulfamethoxazole thiadiazole sulfa methoxy pyridazine, sulfa chlorine pyridazine, sulfonamides 6- (inter) methoxy pyrimidine sulfonamides o-methoxy-ethyl
Piperidine, sulfamethoxazole, sulfamethazine isoxazole, benzoyl sulfonamides, sulfadimethoxine, sulfa quinoline morpholino, hydroxy metronidazole, 2-methyl-5-
Nitroimidazole, hydroxy dimethyl Mi Zun nitrate, metronidazole, Dimetridazole, Ronidazole, chlorine metronidazole imidazole, nitrobenzene and imidazole, hydroxy propyl metronidazole,
Isopropyl metronidazole, marbofloxacin, enoxacin, ofloxacin, norfloxacin, ciprofloxacin, danofloxacin, enrofloxacin, lomefloxacin, Ao Bisha
Star, double difloxacin, sarafloxacin, sparfloxacin, oxolinic acid, nalidixic acid, flumequine, spiramycin, tilmicosin, oleandomycin, tylosin,
Erythromycin, roxithromycin, josamycin, guitar neomycin, tiamulin, lincomycin, clindamycin, pirlimycin and praziquantel residues
Testing.
2 Normative references
The following documents for the application of this document is essential. For dated references, only the dated version suitable for use herein
Member. For undated references, the latest edition (including any amendments) applies to this document.
Laboratory use specifications and test methods GB/T 6682 Analysis
3 PRINCIPLE OF THE METHOD
Pork, shrimp samples were extracted with acetonitrile, hexane, and then the C18 SPE column purification; honey diluted with phosphate buffer solution after
Directly HLB solid phase extraction column purification, liquid chromatography - mass spectrometry/mass spectrometry, quantitative internal standard method or external standard method.
4 Reagents and materials
Unless otherwise indicated, the reagents used were HPLC grade water as a water line with GB/T 6682 regulations.
4.1 acetonitrile.
4.2 methanol.
4.3 formic acid.
4.4 n-hexane.
4.5 anhydrous sodium. AR. 650 ℃ burning 4h, cooled in a desiccator to room temperature and stored in a sealed bottle aside.
4.6 sodium dihydrogen phosphate. AR.
4.7 Sodium hydroxide. AR.
4.8 0.1mol/L sodium hydroxide solution. Weigh 4g of sodium hydroxide, and diluted with water to 1L.
4.9 Phosphate buffer solution. 13.8g of sodium dihydrogen phosphate were dissolved in 950mL water and extracted with 0.1mol/L sodium hydroxide solution to adjust the solution
pH to 8.0, and finally diluted with water to 1L.
4.10 veterinary standards. sulfa drugs purity greater than or equal to 98%, nitroimidazoles purity greater than or equal to 98%, quinolones
Purity of greater than or equal to 96%, macrolides purity of greater than or equal to 95%, lincosamides purity not less than 86% of drug praziquantel
Greater than or equal to 98% purity, detailed criteria for substances listed in Table A.1.
4.11 isotope internal standard Standard. sulfadiazine -D4, Sulfathiazole -D6, sulfapyridine -D6, sulfamethazine -D4, sulfamethoxazole
Oxazole -D6, sulfadimethoxine -D4, sulfa quinoline morpholine -D6, hydroxy dimetridazole -D3, dimetridazole -D3, Ronidazole -D3, hydroxyl
Isopropyl metronidazole -D3, isopropyl metronidazole -D3, enoxacin -D8, ofloxacin -D3, norfloxacin -D5, ciprofloxacin -D8, enrofloxacin -D5,
Double difloxacin -D4, sarafloxacin -D8 isotope standards. purity greater than or equal to 98%, for more information see Table A.1.
4.12 formulated standard stock solution. learn were called commuted right amount standard (4.10) (accurate to 0.1mg), dissolved in methanol to volume,
The concentration of various types of compound solution are 1mg/mL, 1 ℃ ~ 4 ℃ refrigerator stored.
Preparation 4.13 isotope internal standard stock solution. Weigh the right amount of isotope labeled internal standard (4.11), dissolved in methanol to volume, each
The concentration of compound solution are 1mg/mL, 1 ℃ ~ 4 ℃ refrigerator stored.
4.14 intermediate standard solution is prepared by mixing. standard stock solution was diluted with methanol (4.12) to a mixed standard solution containing sulfa final
Drug concentration of 500ng/mL, nitroimidazole drugs at a concentration of 500ng/mL, a concentration of quinolones 1000ng/mL, a large ring
Esters drug concentration of 1500ng/mL, Lim drug concentration amides of 1000ng/mL, praziquantel drug concentration of 150ng/mL,
1 ℃ ~ 4 ℃ refrigerator stored.
4.15 blank sample extract. containing no pork, shrimp or honey sample test drug, in accordance with 7.1 blank sample solutions were prepared.
4.16 matrix mixed standard working solution. a mixed intermediate standard solution (4.14) diluted to fit as needed blank matrix solution (4.15)
Suitable concentrations of mixed standard working solution, using now.
4.17 anhydrous sodium sulfate column. 80mm × 40mm (inner diameter) cylindrical funnel bottom pad 5mm cotton, refill 40mm anhydrous sodium sulfate.
4.18 C18 SPE column. 500mg, 3mL, or rather who, prior to use 5mL methanol pre-wash.
4.19 Oasis (HLB) SPE column, 500mg, 6mL or equivalent person. Before using successively with 5mL methanol, 5mL phosphate buffer
Red solution (4.9) Pre-wash.
4.20 microporous membrane. 0.22μm, organic phase.
5. Apparatus
5.1 Liquid chromatography - mass spectrometry/mass spectrometer. with electrospray ionization (ESI).
5.2 Balance. 0.0001g and a sense of the amount of 0.01g.
5.3 Solid phase extraction device.
5.4 Centrifuge. not less than 6000r/min.
5.5 vortex mixer.
5.6 Instrument concentrated under reduced pressure.
5.7 plug tube. Polypropylene, 50mL.
6 Sample Preparation and Storage
6.1 Preparation and Storage Requirements
In the sample preparation procedure, it should prevent sample contamination or change the content of drug residues occur.
6.2 pork, shrimp
Pork, shrimp sample. Take 500g of representative samples of pork and shrimp, thawed at room temperature, the sample to be broken after all melted, the sample was divided equally
Into two, respectively, into the vial, sealed, marked and labeled. As a test sample, another stored below -18 ℃.
6.3 Honey
Take 500g honey representative sample, the sample will not crystallized its vigorous stirring uniform, crystallized sample vial caps can be plugged
After placed no more than 60 ℃ warm water bath, and other samples were all melted, stir rapidly cooled to room temperature. Should be taken to prevent melting in water
Volatilized. The prepared samples were divided into two, respectively, into the vial, sealed, marked and labeled, stored at room temperature.
7 Procedure
7.1 Extraction and purification
7.1.1 pork, shrimp
Weigh 5g sample (accurate to 0.01g) placed in 50mL stoppered centrifuge tube (5.7), added isotope internal standard solution (sulfa similar position
Su internal standard 8ng, nitroimidazoles isotope internal standard 40ng, quinolones isotope internal standard 30ng), 20mL acetonitrile was added, mixing to
3000r/min centrifugal 3min, the supernatant was transferred to another 50mL stoppered centrifuge tube; the residue was added 15mL of acetonitrile repeat the above operation
For the combined acetonitrile extracts to 7000r/min centrifugal 5min, take the acetonitrile supernatant, 15mL hexane, mixing, 4000r/min
Centrifugal 3min, discard the hexane layer, then add 15mL of n-hexane, repeat the above operation, acetonitrile extract was dried over anhydrous sodium sulfate column (4.17),
At below 40 ℃ water bath evaporated to near dryness and the residue dissolved in methanol was added 4mL quantitatively transferred to a C18 solid phase extraction column (4.18),
Controlling a flow rate of 1mL/min ~ 2mL/min, while receiving the methanol solution was added portionwise 6mL methanol eluate, in
Below 40 ℃ water bath concentrated under reduced pressure to near dryness and 2.0mL of methanol - water (37 volume) constant volume, mix, solution using 0.22μm filter
(4.20) for the liquid chromatography - mass spectrometry/mass spectrometer.
7.1.2 Honey
Weigh 5g sample (accurate to 0.01g) placed in 50mL stoppered centrifuge tube (5.7), added isotope internal standard solution (sulfa similar position
Su internal standard 8ng, nitroimidazoles isotope internal standard 40ng, quinolones isotope internal standard 30ng), plus 20mL phosphate buffer solution
(4.9) dilution, mixing, quantitatively transferred to HLB solid phase extraction column (4.19), controlling the flow rate 1mL/min ~ 2mL/min, discard the effluent,
Add 20mL water rinsed, drained, 6mL methanol eluate, evaporated to near dryness below 40 ℃ water bath, with 2.0mL of methanol -
Water (37 volume) constant volume, mix, solution using 0.22μm filter (4.20), for liquid chromatography - mass spectrometry/mass spectrometer.
7.2 Determination
7.2.1 HPLC conditions
HPLC conditions were as follows.
a) liquid chromatography column. C8,150mm × 4.6mm (diameter), particle size 5μm, or equivalent person;
b) the mobile phase gradient program shown in Table 1;
c) flow rate. 0.8mL/min;
d) Injection volume. 50μL.
Table 1 mobile phase gradient elution table
time
min
Acetonitrile
Methanol
0.15% aqueous formic acid solution
16.5 22078
7.2.2 MS conditions
MS conditions are as follows.
a) ion source. electrospray ion source;
b) scanning. Positive ion scan;
c) detecting mode. multiple reaction monitoring;
d) atomizing gas, air curtain gas, auxiliary gas, collisions are high purity nitrogen gas; the parameters should be adjusted prior to use mass spectrometry to a sensitivity of detection
Requirements, reference conditions and monitoring of ion (m/z) Table B.1.
7.3 Liquid chromatography - mass spectrometry/mass spectrometry
According to the sample tested sample liquid content, similar concentrations of mixed standard solution matrix selected response analyte detection equipment should be
Linear range. Matrix mixed standard solution and sample solution of equal volume is inserted into the sample measured. In the chromatographic conditions of the test from the total drug
Sub chromatogram see Figure C.1, retention time of the reference to Table B.1, standard solution in multiple reaction monitoring chromatogram of the test drug See
Figure C.2 ~ Figure C.6 (detected by this method confirmed the presence of the test drug is recommended to use other methods of quantitative determination again).
7.4 Liquid chromatography - mass spectrometry/mass spectrometry confirmation
Measurement sample matrix and mixed standard working solution in accordance with the above conditions, if the detected peak retention time and mass mixing matrix standard
Working agreed solution, tolerance of less than ± 2.5%. Relative abundance and relative abundance of concentration fairly standard working solution mixed matrix qualitative ion pair
Degree of consistency, the relative abundance of deviation does not exceed the requirements in Table 2, it can determine the presence of the respective analyte in the sample.
Relative ion abundances maximum permissible deviation Table 2% when measured qualitatively
Relative ion abundances > 50 > 20 ~ 50 > 10 ~ 20 ≤10
Relative deviation allowed ± 20 ± 25 ± 30 ± 50
7.5 blank test
Except that no sample addition, according to the above operation steps.
8 Calculation and expression of results
By GC data processor or according to formula (1) calculate the content of an analyte in a sample, the results should be subtracted from the blank value.
Xi = ci × Vm ×
(1)
Where.
Xi --- the amount of analyte in the sample, in micrograms per kilogram (μg/kg);
ci --- the amount of analyte from the sample matrix was mixed on a standard curve obtained in units of nanograms per milliliter (ng/mL);
V --- the final volume of the sample solution, in milliliters (mL);
Sample mass m --- the final sample was representative of the units of grams (g).
9 Determination of lower limit, recovery
9.1 Determination of the lower limit
Lower limit of detection of the standard methods were sulfa drugs 1.0μg/kg, nitroimidazoles 1.0μg/kg, quinolones
2.0μg/kg, macrolides 3.0μg/kg, Lim 2.0μg/kg, praziquantel residues in lactams 0.3μg/kg.
9.2 recoveries
Data recovery and precision test methods (added in different concentration ranges) Table D.1.
Appendix A
(Normative)
Drug Information Standards
Table A.1 Standard Drug Information
No Chinese name English name CAS Number Formula
Relative points
Quality child
Sulfa drugs (16 kinds)
1 Sulfadiazine Sulfadiazine 68-35-9 C10H10N4O2S 250.27
2 Sulfathiazole Sulfathiazloe 72-14-0 C9H9N3O2S2 255.31
3 sulfapyridine Sulfapyridine 144-83-2 C11H11N3O2S 249.28
4 sulfamethyldiazine Sulfamerazine 127-79-7 C11H12N4O2S 264.30
5 sulfamethazine Sulfamethazine 57-68-1 C12H14N4O2S 278.32
6 sulfonamide 5- (p) methoxy pyrimidine Sulfameter 651-06-9 C11H12N4O3S 280.30
7 sulfamethoxazole thiadiazole Sulfamethizole 144-82-1 C9H10N4O2S2 270.32
8 sulfa methoxy pyridazine Sulfamethoxypyridazine 80-35-3 C11H12N4O3S 280.30
9 sulfa-chloro pyridazine Sulfachloropyridazine 80-32-0 C10H9ClN4O2S 284.72
10 sulfonamide-6- (inter) methoxy pyrimidine Sulfamonomethoxine 1220-83-3 C11H12N4O3S 280.30
11 o-methoxy pyrimidine sulfonamides Sulfadoxine 2447-57-6 C12H14N4O4S 310.32
12 sulfamethoxazole Sulfamethoxazole 723-46-6 C10H11N3O3S 253.27
13 sulfamethazine isoxazole Sulfafurazole 127-69-5 C11H13N3O3S 267.30
14 benzoyl sulfonamide Sulfabenzamide 127-71-9 C13H12N2O3S 276.31
15 Sulfadimethoxine Sulfadimethoxine 122-11-2 C12H14N4O4S 310.32
16 sulfa quinoline morpholine Sulfaquinoxaline 59-40-5 C14H12N4O2S 300.33
Sulfadiazine -D4 Sulfadiazine-D4 1020719-78-1 C10H6D4N4O2S 254.30
Sulfathiazole -D6 Sulfathiazole-D6 C9H3D6N3O2S2 261.05
SASP -D6 Sulfapyridine-D6 C11H5D6N3O2S 255.09
Sulfamethazine -D4 Sulfamethazine-D4 C12H10D4N4O2S 282.36
Sulfamethoxazole -D6 Sulfamethoxazole-D6 C10H5D6N3O3S 259.09
Sulfadimethoxine -D4 Sulfadimethoxine-D4 C12H10D4N4O4S 314.35
Sulfa quinoline morpholine -D6 Sulfaquinoxaline-D6 C14H6D6N4O2S 306.11
Nitroimidazoles (10 kinds)
17-hydroxy-metronidazole
1- (2-Hydroxyethyl) -2-
hydroxy-methyl-5-nitr
oimidazol (MNZOH)
4812-40-2 C6H9N3O4 187.15
182--methyl-5-nitro-imidazol-2-Methyl-5-nitroimidazole 88054-22-2 C4H5N3O2 127.10
Table A.1 (CONTINUED)
No Chinese name English name CAS Number Formula
Relative points
Quality child
19-hydroxy dimetridazole
2-Hydroxymethyl-1-
methyl-5-nitroimidazo
le (DMZOH, HMMNI)
936-05-0 C5H7N3O3 157.13
20 Metronidazole Metronidazole (MNZ) 443-48-1 C6H9N3O3 171.15
21 Dimetridazole Dimetridazole (DMZ) 551-92-8 C5H7N3O2 141.13
22 Ronidazole Ronidazole (RNZ) 7681-76-7 C6H8N4O4 200.15
23 chlorine metronidazole imidazole
5-Chloro-1-methyl-4-
nitroimidazole
4897-25-0 C4H4ClN3O2 161.55
24 benzene imidazole nitrate 5-Nitrobenzimidazo1e 94-52-0 C7H5N3O2 163.14
25-hydroxy-propyl metronidazole Ipronidazole-OH (IPZOH) 35175-14-5 C7H11N3O3 185.18
26 isopropyl metronidazole Ipronidazole (IPZ) 14885-29-1 C7H11N3O2 169.18
Hydroxy Dimetridazole -D3 DMZOH-D3 C5H4D3N3O3 160.2
Dimetridazole -D3 DMZ-D3 C5H4D3N3O2 144.2
Ronidazole -D3 RNZ-D3 C6H5D3N4O4 203.2
Hydroxy propyl metronidazole -D3 IPZOH-D3 C7H8D3N3O3 188.2
Isopropyl metronidazole -D3 IPZ-D3 C7H8D3N3O2 172.2
Quinolones (15 kinds)
27 marbofloxacin Marbofloxacin 115550-35-1 C17H19FN4O4 362.36
28 enoxacin Enoxacin 74011-58-8 C15H17FN4O3 320.32
29 ofloxacin Ofloxacin 82419-36-1 C18H20FN3O4 361.37
30 norfloxacin Norfloxacin 70458-96-7 C16H18FN3O3 319.33
31 Ciprofloxacin Ciprofloxacinhydrochloride 86393-32-0 C17H18FN3O3HCl 367.81
32 danofloxacin Danofloxacinmesylate 119478-55-6 C20H24FN3O6S 453.6
33 enrofloxacin Enrofloxacine 93106-60-6 C19H22FN3O3 359.4
34 lomefloxacin
Lomefloxacin
hydrochloride
98079-52-8 C17H19F2N3O3HCl 387.8
35 Orbifloxacin Orbifloxacin 113617-63-3 C19H20F3N3O3 395.38
36 pairs Difloxacin Difloxacin 98106-17-3 C21H19F2N3O3 400.16
37 Sarafloxacin
Sarafloxacin
hydrochloride
98105-99-8 C20H17F2N3O3HCl 421.83
38 sparfloxacin Sparfloxacin 111542-93-9 C19H22F2N4O3 392.40
39 quinoline acid Oxolinicacid 14698-29-4 C13H11NO5 261.23
40 nalidixic acid Nalidixicacid 389-08-2 C12H12N2O3 232.23
41 Flumequine Flumequine 42835-25-6 C14H12FNO3 261.25
Enoxacin -D8 Enoxacin-D8 C15H9D8FN4O3 328.18
Table A.1 (CONTINUED)
No Chinese name English name CAS Number Formula
Relative points
Quality child
Ofloxacin -D3 Ofloxacin-D3 C18H17D3FN3O4 364.16
Norfloxacin -D5 Norfloxacin-D5 C16H13D5FN3O3 324.33
Ciprofloxacin -D8 Ciprofloxacin-D8 C17H10D8FN3O3 339.81
Enrofloxacin -D5 Enrofloxacine-D5 C19H17D5FN3O3 364.20
Double difloxacin -D4 Difloxacin-D4 C21H15D4F2N3O3 403.16
Sarafloxacin -D8 Sarafloxacin-D8 C20H9D8F2N3O3 393.17
Macrolides (nine kinds)
42 Spiramycin Spiramycin 8025-81-8 C43H74N2O14 843.06
43 Tilmicosin Tilmicosin 108050-54-0 C46H80N2O13 869.13
44 oleandomycin phosphate
Oleandomycin
phosphate
7060-74-4 C35H61NO12H3PO4 · 2H2O 687.4
45 tylosin tartrate Tylosintartrate 74610-55-2 C50H83NO23 915.5
46 erythromycin A dihydrate Erythromycin 59319-72-1 C37H67NO13 733.9
47 Roxithromycin Roxithromycin 80214-83-1 C41H76N2O15 837.0
48 josamycin Josamycin 16846-24-5 C42H69NO15 827.9
49 kitasamycin Kitasamycin 1392-21-8 C39H65NO14 771.93
50 Tiamulin Tiamulin 55297-95-5 C28H47NO4S 493.74
Lincosamides drugs (three kinds)
51 Lincomycin hydrochloride
Lincomycin
hydrochloride
monhydrate
859-18-7 C18H34N2O6S · HCl 443.0
52 clindamycin hydrochloride
C1indamycin
hydrochloride
21462-39-5 C18H33ClN2O5S · HCl 461.4
53 pirlimycin hydrochloride
Pirlimycin
hydrochloride
79548-73-5 C17H31ClN2O5S · HCl 446.0
54 topiramate wow ketone Praziquantel 55268-74-1 C19H24N2O2 312.41
Appendix B
(Informative)
APl4000LC-MS/MS system electrospray ionization source reference conditions 1)
API4000LC-MS/MS system electrospray ionization source reference conditions.
a) electrospray voltage (IS). 5500V.
b) atomizing air pressure (GS1). 358.28kPa (52psi);
c) air curtain air pressure (CUR). 172.25kPa (25psi);
d) auxiliary gas flow rate (GS2). 378.95kPa (55psi);
e) ion source temperature (TEM). 550 ℃;
f) Collision gas (CAD). 6;
g) ions on quantitative and qualitative ion pairs to cluster voltage (DP), air collision energy (CE), the collision chamber outlet voltage (CXP) and relative security
Retention time shown in Table B.1.
Table B.1 ions on quantitative and qualitative ion pairs to cluster voltage, gas energy collision, the collision chamber outlet voltage and retention time
Compound
Ion pair
m/z
To cluster voltage
(DP)
Air collision
Energy (CE)
Collision chamber outlet
Voltage (CXP)
Internal standard compound
keep time
min
1 sulfadiazine
251.1/156.3 *
251.1/108.2
twenty two
10 sulfadiazine -D4 4.35
2 Sulfathiazole
255.8/156.3 *
255.8/108.2
twenty two
10 Sulfathiazole -D6 4.90
3 SASP
249.9/156.2 *
249.9/184.4
702 410 SASP -D6 5.29
4 sulfamethyldiazine
265.1/156.3 *
265.1/172.2
twenty three
10 sulfadiazine -D4 6.06
5 sulfamethazine
279.2/156.3 *
279.2/186.1
702 610 sulfamethazine -D4 7.78
Sulfonamide 5- (p)
Methoxy pyrimidine
281.2/156.3 *
281.2/215.4
10 sulfamethazine -D4 8.35
7 sulfamethoxazole thiadiazole
271.0/156.2 *
271.0/108.2
twenty four
10 sulfamethazine -D4 8.75
8 sulfa methoxy pyridazine
281.2/156.3 *
281.2/215.4
10 sulfamethazine -D4 9.29
9 sulfa-chloro pyridazine
285.0/156.3 *
285.0/108.2
twenty two
10 sulfadimethoxine -D4 11.5
Sulfa-6- (room) methoxy
Pyrimidine
281.2/156.3 *
281.2/215.4
10 sulfamethazine -D4 11.9
1) non-commercial declared. parameters listed in Table B.1 in API4000 mass spectrometer, the test instrument models listed here only for reference and
Not involved in commercial purposes, to encourage users to try different standard manufacturers and models of equipment.
Table B.1 (continued)
Compound
Ion pair
m/z
To cluster voltage
(DP)
Air collision
Energy (CE)
Collision chamber outlet
Voltage (CXP)
Internal standard compound
keep time
min
11 o-methoxy pyrimidine sulfonamides
311.2/156.3 *
311.2/108.2
10 sulfadimethoxine -D4 12.1
12 sulfamethoxazole
254.1/156.3 *
254.1/108.2
twenty two
10 sulfamethoxazole -D6 12.1
13 sulfamethazine isoxazole
268.0/156.3 *
268.0/113.2
702 210 sulfadimethoxine -D4 12.5
14 benzoyl sulfonamide
277.0/156.2 *
277.0/92.0
Sulfadimethoxine -D4 12.8
15 sulfadimethoxine
311.2/156.3 *
311.2/108.2
10 sulfadimethoxine -D4 13.1
16 sulfa quinoline morpholine
301.2/156.3 *
301.2/108.2
twenty four
Sulfa quinoline morpholine -D6 13.1
Sulfadiazine -D4 255.2/160.3 56 22 12
Sulfathiazole -D6 262.0/97.9 72 39 8
SASP -D6 256.2/97.9 70 38 7...
...
