Article(id=1220364157635973314, tenantId=1146029695717560320, journalId=1189982191388893191, issueId=1220364151428403238, articleNumber=null, orderNo=null, doi=10.16438/j.0513-4870.2019-0531, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1562256000000, receivedDateStr=2019-07-05, revisedDate=1566316800000, revisedDateStr=2019-08-21, acceptedDate=null, acceptedDateStr=null, onlineDate=1768887088449, onlineDateStr=2026-01-20, pubDate=1578758400000, pubDateStr=2020-01-12, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1768887088449, onlineIssueDateStr=2026-01-20, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1768887088449, creator=13701087609, updateTime=1768887088449, updator=13701087609, issue=Issue{id=1220364151428403238, tenantId=1146029695717560320, journalId=1189982191388893191, year='2020', volume='55', issue='1', pageStart='1', pageEnd='180', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1768887086970, creator=13701087609, updateTime=1768887655045, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1220366534166365022, tenantId=1146029695717560320, journalId=1189982191388893191, issueId=1220364151428403238, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1220366534166365023, tenantId=1146029695717560320, journalId=1189982191388893191, issueId=1220364151428403238, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=113, endPage=122, ext={EN=ArticleExt(id=1220364160907530474, articleId=1220364157635973314, tenantId=1146029695717560320, journalId=1189982191388893191, language=EN, title=Qualitative screening of 169 veterinary drug residues in bear bile powder by QuEChERS-ultra high performance liquid chromatography-tandem mass spectrometry, columnId=1190335348648547107, journalTitle=Acta Pharmaceutica Sinica, columnName=Reviews, runingTitle=null, highlight=null, articleAbstract=

A QuEChERS-ultra high performance liquid chromatography-tandem mass spectrometry method was developed for qualitative screening of 169 veterinary drug residues in bear bile powder, including β-agonists and inhibitors, antibiotics (penicillins, β-lactams, sulfomamides, quinolones, chloramphenicals, tetracyclines, nitroimidazoles, macrolides, polyethers, etc.), antiviral drugs, anthelminitics, steroid hormones, nonsteroidal antiinflammatory drugs (NSAIDs) and sedatives. The samples were extracted by Na2EDTA-McIlvaine buffer solution and 5% fomic acid-acetonitrile solution, then purified by dispersive solid phase extraction. Detection of veterinary drug residues by ultra high performance liquid chromatography-triple quadrupole mass spectrometry was conducted and qualitative confirmed by ion ratios. The limits of detection of 169 veterinary drugs were 1-1 000 μg·kg-1. The method is simple and fast, which had been used for the analysis of actual samples, and can be extended to the detection of similar matrix.

, correspAuthors=Shen JI, authorNote=null, correspAuthorsNote=null, copyrightStatement=Copyright ©2020 Acta Pharmaceutica Sinica. All rights reserved., copyrightOwner=null, extLink=null, articleAbsUrl=null, sourceXml=null, magXml=null, pdfUrl=null, pdf=null, pdfFileSize=null, pdfExtLink=null, richHtmlUrl=null, mobilePdfUrl=null, reviewReport=null, pdfFirstPage=null, abstractGraph=null, abstractGraphContent=null, abstractVideo=null, citation=null, cebUrl=null, magXmlContent=null, mapNumber=null, authorCompany=null, fund=null, authors=null, authorsList=Jian SUN, Qing HU, Yan-rong ZHU, Su ZHANG, Hong YU, Rui FENG, Jing-xian ZHANG, Xiu-hong MAO, Shen JI), CN=ArticleExt(id=1220364163424112958, articleId=1220364157635973314, tenantId=1146029695717560320, journalId=1189982191388893191, language=CN, title=QuEChERS-超高效液相色谱串联质谱法定性筛查中药材熊胆粉中169种兽药残留, columnId=1190335348896011050, journalTitle=药学学报, columnName=研究论文, runingTitle=null, highlight=null, articleAbstract=

建立了QuEChERS-超高效液相色谱串联质谱法定性筛查中药材熊胆粉中多种兽药残留,包括β-受体激动剂与拮抗剂、抗生素(青霉素类、头孢菌素类、磺胺类、喹诺酮类、氯霉素类、四环素类、硝基咪唑类、大环内酯类、聚醚类等)、抗病毒药、驱虫药、甾体激素、非甾体抗炎药和镇静剂等169种兽药残留。样品经Na2EDTA-McIlvaine缓冲液和5%甲酸乙腈提取,经分散固相萃取法净化,以超高效液相色谱串联三重四极杆质谱法测定,通过离子丰度比定性判定。169种化合物检出限为1~1 000 μg·kg-1。本方法简便快速,已应用于实际样品的测定,并可扩展至其他类似药材基质的检测。

, correspAuthors=季申, authorNote=null, correspAuthorsNote=
*季申, Tel:86-21-50798195, E-mail:
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Category Compound CAS No. Solvent LOD/μg·kg-1
β-Agonists Cimaterol 54239-37-1 a 10
Clorprenaline 3811-25-4 a 10
Terbutaline 23031-32-5 a 1
Tulobuterol 56776-01-3 a 1
Clenbuterol 21898-19-1 a 10
Penbutolol 28163-36-2 a 10
Ractopamine 90274-24-1 a 1
Salbutamol 18559-94-9 a 1
β-Inhibitors Propanolol 318-98-9 a 100
Carazolol 57775-29-8 b 1
Penicillins Ampicillin 69-53-4 c 50
Oxacillin 66-79-5 c 250
Piperacillin 61477-96-1 c 10
Sulbactam 68373-14-8 c 50
Cloxacillin 7081-44-9 c 50
Dicloxacillin 13412-64-1 c 50
Penicilline V 132-98-9 c 50
Penicilline G 61-33-6 a 50
β-Lactams Cefapirin 21593-23-7 c 10
Cefazolin 25953-19-9 c 10
Cefetamet pivoxyl 65243-33-6 c 10
Cefotaxime 63527-52-6 c 10
Ceftiofur 80370-57-6 c 10
Cephalonium 5575-21-3 c 10
Cefamandole 58648-57-0 c 50
Cefoperazone 62893-20-3 c 10
Cefquinome 118443-89-3 c 10
Sulfomamides Sulfabenzamide 127-71-9 a 1
Sulfacetamide 144-80-9 a 1
Sulfachloropyridazine 80-32-0 a 1
Sulfaclozine 102-65-8 a 50
Sulfadimethoxine 122-11-2 a 1
Sulfaguanidine 57-67-0 a 1
Sulfamerazine 127-79-7 a 1
Sulfamethizole 144-82-1 a 1
Sulfamethoxazole 723-46-6 a 5
Sulfamonomethoxine 1220-83-3 a 1
Sulfamoxole 729-99-7 a 1
Sulfaphenazole 526-08-9 a 50
Sulfapyridine 144-83-2 a 1
Sulfaquinoxaline 59-40-5 a 1
Sulfathiazole 72-14-0 a 10
Sulphisoxazole 127-69-5 a 10
Sulfadiazine 68-35-9 a 1
Sulfamethazine 57-68-1 a 1
Sulfadoxine 2447-57-6 a 1
Sulfameter 651-06-9 a 1
Sulfamethoxypyridazine 80-35-3 a 10
Sulfisomidine 515-64-0 a 10
Trimethoprim 738-70-5 a 10
Quinolones Ciprofloxacin 85721-33-1 d 100
Danofloxacin 112398-08-0 d 50
Difloxacin 98106-17-3 d 50
Enoxacin 74011-58-8 d 250
Enrofloxacin 93106-60-6 d 10
Fleroxacin 79660-72-3 d 10
Lomefloxacin 98079-51-7 d 50
Nalidixic acid 389-08-2 d 10
Norfloxacin 70458-96-7 d 500
Ofloxacin 82419-36-1 d 100
Orbifloxacin 113617-63-3 d 1
Oxolinic acid 14698-29-4 d 10
Pefloxacin 70458-92-3 d 100
Sarafloxacin 98105-99-8 d 50
Sparfloxacin 110871-86-8 d 50
Flumequine 42835-25-6 d 10
Marbofloxacin 115550-35-1 a 10
Nequinate 13997-19-8 e 1
Chloramphenicals Chloramphenicol 56-75-7 a 10
Florfenicol 73231-34-2 a 10
Thiamphenicol 15318-45-3 a 10
Tetracyclines Oxytetracycline 2058-46-0 a 100
Tetracycline 60-54-8 a 500
Chlortetracycline 64-72-2 a 100
Doxycycline 24390-14-5 a 1 000
Nitroimidazoles Metronidazole 443-48-1 a 100
Hydroxydimetridazole 936-05-0 a 100
Hydroxymetronidazole 4812-40-2 a 10
Dimetridazole 551-92-8 a 100
Ronidazole 7681-76-7 a 10
Macrolides Erythromycin 114-07-8 a 10
Oleandomycin 7060-74-4 a 10
Tylosin 1401-69-0 a 1
Tylvalosin 63428-13-7 a 10
Avermectin B1a 71751-41-2 a 50
Doramectin 117704-25-3 a 10
Eprinomectin B1a 123997-26-2 a 50
Ivermectin B1a 70288-86-7 a 10
Kitasamycin 1392-21-8 a 10
Polyethers Maduramicin 84878-61-5 a 1
Monensin 22373-78-0 a 1
Nigericin 28643-80-3 a 10
Other antibiotics Dapson 80-08-0 a 1
N-Acetyl dapson 565-20-8 a 1
Lincomycin 859-18-7 a 10
Valnemulin 133868-46-9 a 10
Olaquindox 23696-28-8 f 500
3-Methyl-quinoxaline-2-carboxylic acid 74003-63-7 f 500
Antiviral drugs Amantadine 768-94-5 a 250
Anthelminitics 2-Aminoflubendazole 82050-13-3 g 1
5-Hydroxymebendazole 60254-95-7 g 1
Albendazole 54965-21-8 g 1
Albendazole sulfone 75184-71-3 g 10
Albendazole sulfoxide 54029-12-8 g 1
Cambendazole 26097-80-3 g 1
Fenbendazole 43210-67-9 g 1
Flubendazole 31430-15-6 g 1
Mebendazole 31431-39-7 g 1
Oxfendazole 53716-50-0 g 1
Oxfendazole sulfone 54029-20-8 g 1
Oxibendazole 20559-55-1 g 1
Thiabendazole 148-79-8 g 10
Triclabendazole 68786-66-3 g 10
Hydroxy-thiabendazole 948-71-0 g 10
Mebendazole-amine 52329-60-9 g 10
Clopidol 2971-90-6 a 10
Diclazuril 101831-37-2 a 1
Ethopabate 1959/6/3 a 1
Febantel 58306-30-2 a 1
Nitroxynil 1689-89-0 a 10
Zoalene 148-01-6 a 10
Halofuginone 64924-67-0 a 50
Levamisole 16595-80-5 a 50
Nicarbazine 330-95-0 a 1
Basic violet 3 548-62-9 h 1
Robenidine 25875-50-7 a 10
Leucomalachite green 129-73-7 a 1
Steroid hormones Betamethasone 378-44-9 b 10
Dexamethasone 1950/2/2 b 10
Flumethasone 2135-17-3 b 50
Hydrocortisone 50-23-7 b 100
Methylprednisolone 83-43-2 b 10
Prednisolone 50-24-8 b 100
Prednisone 1953/3/2 b 100
Triamcinolone 124-94-7 b 1
Triamcinolone acetonide 76-25-5 b 10
Fludrocortisone acetate 514-36-3 b 250
Cortisone acetate 1950/4/4 b 500
Testosterone 58-22-0 b 50
Testosterone propionate 57-85-2 b 50
Methyltestosterone 58-18-4 b 50
Nandrolone phenlpropionate 62-90-8 b 100
Trenbolone 10161-33-8 b 100
Progesterone 57-83-0 b 50
Megestrol acetate 595-33-5 b 10
Melengestrol acetate 2919-66-6 b 50
Chlormadinone acetate 302-22-7 b 10
NSAIDs 4-Acetamido antipyrine 83-15-8 b 1
4-Formylamino antipyrine 1672-58-8 b 1
Carprofen 53716-49-7 b 100
Diclofenac 15307-86-5 b 10
Indomethacin 53-86-1 b 50
Indoprofen 31842-01-0 b 10
Mefenamic acid 61-68-7 b 1
Meloxicam 71125-38-7 b 10
Piroxicam 36322-90-4 b 50
Sulindac 38194-50-2 b 10
Tenoxicam 59804-37-4 b 10
Tolfenamic acid 13710-19-5 b 250
Tolmetin 26171-23-3 b 10
Sedatives Acepromazine 3598-37-6 b 1
Azaperol 2804/5/9 b 10
Azaperone 1649-18-9 b 1
Chlorpromazine 69-09-0 b 10
Diazepam 439-14-5 a 10
Haloperidol 52-86-8 b 1
Methaqualone 72-44-6 a 100
Propionylpromazine 7681-67-6 b 10
Xylazine 7361-61-7 a 1
), ArticleFig(id=1220364172676747991, tenantId=1146029695717560320, journalId=1189982191388893191, articleId=1220364157635973314, language=CN, label=Table 1, caption=

Information of the 169 reference compounds and LODs. a: Methanol; b: Acetonitrile; c: 25% Acetonitrile; d: 1% Formic acid-methanol; e: Methanol-dichloromethane (4:1); f: Methanol-water-acetonitrile (7:2:1); g: Acetonitrile-methanol (1:1); h: 1% Formic acid-acetonitrile

, figureFileSmall=null, figureFileBig=null, tableContent=
Category Compound CAS No. Solvent LOD/μg·kg-1
β-Agonists Cimaterol 54239-37-1 a 10
Clorprenaline 3811-25-4 a 10
Terbutaline 23031-32-5 a 1
Tulobuterol 56776-01-3 a 1
Clenbuterol 21898-19-1 a 10
Penbutolol 28163-36-2 a 10
Ractopamine 90274-24-1 a 1
Salbutamol 18559-94-9 a 1
β-Inhibitors Propanolol 318-98-9 a 100
Carazolol 57775-29-8 b 1
Penicillins Ampicillin 69-53-4 c 50
Oxacillin 66-79-5 c 250
Piperacillin 61477-96-1 c 10
Sulbactam 68373-14-8 c 50
Cloxacillin 7081-44-9 c 50
Dicloxacillin 13412-64-1 c 50
Penicilline V 132-98-9 c 50
Penicilline G 61-33-6 a 50
β-Lactams Cefapirin 21593-23-7 c 10
Cefazolin 25953-19-9 c 10
Cefetamet pivoxyl 65243-33-6 c 10
Cefotaxime 63527-52-6 c 10
Ceftiofur 80370-57-6 c 10
Cephalonium 5575-21-3 c 10
Cefamandole 58648-57-0 c 50
Cefoperazone 62893-20-3 c 10
Cefquinome 118443-89-3 c 10
Sulfomamides Sulfabenzamide 127-71-9 a 1
Sulfacetamide 144-80-9 a 1
Sulfachloropyridazine 80-32-0 a 1
Sulfaclozine 102-65-8 a 50
Sulfadimethoxine 122-11-2 a 1
Sulfaguanidine 57-67-0 a 1
Sulfamerazine 127-79-7 a 1
Sulfamethizole 144-82-1 a 1
Sulfamethoxazole 723-46-6 a 5
Sulfamonomethoxine 1220-83-3 a 1
Sulfamoxole 729-99-7 a 1
Sulfaphenazole 526-08-9 a 50
Sulfapyridine 144-83-2 a 1
Sulfaquinoxaline 59-40-5 a 1
Sulfathiazole 72-14-0 a 10
Sulphisoxazole 127-69-5 a 10
Sulfadiazine 68-35-9 a 1
Sulfamethazine 57-68-1 a 1
Sulfadoxine 2447-57-6 a 1
Sulfameter 651-06-9 a 1
Sulfamethoxypyridazine 80-35-3 a 10
Sulfisomidine 515-64-0 a 10
Trimethoprim 738-70-5 a 10
Quinolones Ciprofloxacin 85721-33-1 d 100
Danofloxacin 112398-08-0 d 50
Difloxacin 98106-17-3 d 50
Enoxacin 74011-58-8 d 250
Enrofloxacin 93106-60-6 d 10
Fleroxacin 79660-72-3 d 10
Lomefloxacin 98079-51-7 d 50
Nalidixic acid 389-08-2 d 10
Norfloxacin 70458-96-7 d 500
Ofloxacin 82419-36-1 d 100
Orbifloxacin 113617-63-3 d 1
Oxolinic acid 14698-29-4 d 10
Pefloxacin 70458-92-3 d 100
Sarafloxacin 98105-99-8 d 50
Sparfloxacin 110871-86-8 d 50
Flumequine 42835-25-6 d 10
Marbofloxacin 115550-35-1 a 10
Nequinate 13997-19-8 e 1
Chloramphenicals Chloramphenicol 56-75-7 a 10
Florfenicol 73231-34-2 a 10
Thiamphenicol 15318-45-3 a 10
Tetracyclines Oxytetracycline 2058-46-0 a 100
Tetracycline 60-54-8 a 500
Chlortetracycline 64-72-2 a 100
Doxycycline 24390-14-5 a 1 000
Nitroimidazoles Metronidazole 443-48-1 a 100
Hydroxydimetridazole 936-05-0 a 100
Hydroxymetronidazole 4812-40-2 a 10
Dimetridazole 551-92-8 a 100
Ronidazole 7681-76-7 a 10
Macrolides Erythromycin 114-07-8 a 10
Oleandomycin 7060-74-4 a 10
Tylosin 1401-69-0 a 1
Tylvalosin 63428-13-7 a 10
Avermectin B1a 71751-41-2 a 50
Doramectin 117704-25-3 a 10
Eprinomectin B1a 123997-26-2 a 50
Ivermectin B1a 70288-86-7 a 10
Kitasamycin 1392-21-8 a 10
Polyethers Maduramicin 84878-61-5 a 1
Monensin 22373-78-0 a 1
Nigericin 28643-80-3 a 10
Other antibiotics Dapson 80-08-0 a 1
N-Acetyl dapson 565-20-8 a 1
Lincomycin 859-18-7 a 10
Valnemulin 133868-46-9 a 10
Olaquindox 23696-28-8 f 500
3-Methyl-quinoxaline-2-carboxylic acid 74003-63-7 f 500
Antiviral drugs Amantadine 768-94-5 a 250
Anthelminitics 2-Aminoflubendazole 82050-13-3 g 1
5-Hydroxymebendazole 60254-95-7 g 1
Albendazole 54965-21-8 g 1
Albendazole sulfone 75184-71-3 g 10
Albendazole sulfoxide 54029-12-8 g 1
Cambendazole 26097-80-3 g 1
Fenbendazole 43210-67-9 g 1
Flubendazole 31430-15-6 g 1
Mebendazole 31431-39-7 g 1
Oxfendazole 53716-50-0 g 1
Oxfendazole sulfone 54029-20-8 g 1
Oxibendazole 20559-55-1 g 1
Thiabendazole 148-79-8 g 10
Triclabendazole 68786-66-3 g 10
Hydroxy-thiabendazole 948-71-0 g 10
Mebendazole-amine 52329-60-9 g 10
Clopidol 2971-90-6 a 10
Diclazuril 101831-37-2 a 1
Ethopabate 1959/6/3 a 1
Febantel 58306-30-2 a 1
Nitroxynil 1689-89-0 a 10
Zoalene 148-01-6 a 10
Halofuginone 64924-67-0 a 50
Levamisole 16595-80-5 a 50
Nicarbazine 330-95-0 a 1
Basic violet 3 548-62-9 h 1
Robenidine 25875-50-7 a 10
Leucomalachite green 129-73-7 a 1
Steroid hormones Betamethasone 378-44-9 b 10
Dexamethasone 1950/2/2 b 10
Flumethasone 2135-17-3 b 50
Hydrocortisone 50-23-7 b 100
Methylprednisolone 83-43-2 b 10
Prednisolone 50-24-8 b 100
Prednisone 1953/3/2 b 100
Triamcinolone 124-94-7 b 1
Triamcinolone acetonide 76-25-5 b 10
Fludrocortisone acetate 514-36-3 b 250
Cortisone acetate 1950/4/4 b 500
Testosterone 58-22-0 b 50
Testosterone propionate 57-85-2 b 50
Methyltestosterone 58-18-4 b 50
Nandrolone phenlpropionate 62-90-8 b 100
Trenbolone 10161-33-8 b 100
Progesterone 57-83-0 b 50
Megestrol acetate 595-33-5 b 10
Melengestrol acetate 2919-66-6 b 50
Chlormadinone acetate 302-22-7 b 10
NSAIDs 4-Acetamido antipyrine 83-15-8 b 1
4-Formylamino antipyrine 1672-58-8 b 1
Carprofen 53716-49-7 b 100
Diclofenac 15307-86-5 b 10
Indomethacin 53-86-1 b 50
Indoprofen 31842-01-0 b 10
Mefenamic acid 61-68-7 b 1
Meloxicam 71125-38-7 b 10
Piroxicam 36322-90-4 b 50
Sulindac 38194-50-2 b 10
Tenoxicam 59804-37-4 b 10
Tolfenamic acid 13710-19-5 b 250
Tolmetin 26171-23-3 b 10
Sedatives Acepromazine 3598-37-6 b 1
Azaperol 2804/5/9 b 10
Azaperone 1649-18-9 b 1
Chlorpromazine 69-09-0 b 10
Diazepam 439-14-5 a 10
Haloperidol 52-86-8 b 1
Methaqualone 72-44-6 a 100
Propionylpromazine 7681-67-6 b 10
Xylazine 7361-61-7 a 1
), ArticleFig(id=1220364172785799902, tenantId=1146029695717560320, journalId=1189982191388893191, articleId=1220364157635973314, language=EN, label=null, caption=null, figureFileSmall=null, figureFileBig=null, tableContent=
No. Compound Precursor ion (m/z) Product ion (m/z) CE/V Ionization mode RT/min
1 2-Aminoflubendazole 256.1 123.0, 95.0 40, 40 [M+H]+ 8.04
2 3-Methyl-quinoxaline-2-carboxylic acid 189.1 145.0, 143.0 12, 16 [M+H]+ 5.38
3 4-Acetamido antipyrine 246.1 227.9, 83.0 12, 40 [M+H]+ 4.76
4 4-Formylamino antipyrine 232.1 104.0, 83.0 20, 20 [M+H]+ 4.79
5 5-Hydroxymebendazole 298.1 266.1, 79.1 25, 44 [M+H]+ 7.64
6 Acepromazine 327.2 86.1, 58.1 20, 48 [M+H]+ 11.74
7 Albendazole 266.1 234.1, 191.0 16, 32 [M+H]+ 12.75
8 Albendazole sulfone 298.1 266.1, 159.0 20, 40 [M+H]+ 8.50
9 Albendazole sulfoxide 282.1 239.9, 208.0 12, 24 [M+H]+ 6.31
10 Amantadine 152.1 135.0, 77.1 18, 50 [M+H]+ 5.18
11 Ampicillin 350.0 114.0, 106.0 36, 16 [M+H]+ 4.42
12 Avermectin B1a 895.5 751.4, 449.3 48, 48 [M+Na]+ 18.02
13 Azaperol 330.2 312.1, 121.0 16, 20 [M+H]+ 5.94
14 Azaperone 328.2 165.1, 121.1 20, 20 [M+H]+ 7.03
15 Basic violet 3 372.3 356.1, 340.0 44, 55 [M+H]+ 15.01
16 Betamethasone 393.2 373.2, 355.2 4, 8 [M+H]+ 13.01
17 Cambendazole 303.1 261.0, 217.1 16, 32 [M+H]+ 8.34
18 Carazolol 299.2 222.0, 116.0 20, 20 [M+H]+ 8.54
19 Carprofen 272.0 227.9, 225.9 12, 28 [M-H]- 15.16
20 Cefamandole 463.1 347.0, 158.0 4, 16 [M+H]+ 8.05
21 Cefapirin 424.1 291.9, 151.9 12, 28 [M+H]+ 3.74
22 Cefazolin 455.0 323.0, 156.0 8, 11 [M+H]+ 5.58
23 Cefetamet pivoxyl 512.1 241.0, 57.1 16, 48 [M+H]+ 14.23
24 Cefoperazone 646.2 530.2, 143.0 8, 45 [M+H]+ 7.21
25 Cefotaxime 456.1 324.0, 125.0 8, 60 [M+H]+ 5.11
26 Cefquinome 529.1 134.2, 125.0 8, 60 [M+H]+ 4.39
27 Ceftiofur 524.0 241.0, 126.0 16, 40 [M+H]+ 9.22
28 Cephalonium 459.1 337.0, 152.0 8, 20 [M+H]+ 4.82
29 Chloramphenicol 321.0 152.1, 121.0 14, 36 [M-H]- 9.19
30 Chlorpromazine 319.1 86.1, 58.2 16, 44 [M+H]+ 13.66
31 Chlortetracycline 479.1 444.0, 154.1 20, 36 [M+H]+ 7.95
32 Chlormadinone acetate 405.2 345.0, 309.0 12, 16 [M+H]+ 16.12
33 Cimaterol 220.1 202.1, 143.1 4, 20 [M+H]+ 3.57
34 Ciprofloxacin 332.1 314.0, 231.0 20, 48 [M+H]+ 5.23
35 Clenbuterol 277.1 259.1, 203.0 4, 12 [M+H]+ 6.75
36 Clopidol 192.1 101.0, 51.0 25, 48 [M+H]+ 4.23
37 Clorprenaline 214.1 196.0, 153.9 8, 12 [M+H]+ 5.62
38 Cloxacillin 436.0 277.0, 160.0 12, 12 [M+H]+ 14.00
39 Cortisone acetate 403.2 343.1, 163.0 20, 28 [M+H]+ 14.28
40 Danofloxacin 358.2 340.1, 82.1 20, 48 [M+H]+ 5.56
41 Dapson 249.1 156.0, 92.0 10, 28 [M+H]+ 7.25
42 Dexamethasone 393.2 373.2, 355.2 2, 6 [M+H]+ 12.88
43 Diazepam 285.1 193.1, 153.9 37, 29 [M+H]+ 14.91
44 Diclazuril 405.0 334.8, 334.0 16, 20 [M-H]- 15.58
45 Diclofenac 296.0 215.1, 214.1 16, 48 [M+H]+ 15.45
46 Dicloxacillin 470.0 310.8, 159.9 12, 12 [M+H]+ 14.53
47 Difloxacin 400.1 356.2, 299.1 16, 32 [M+H]+ 6.92
48 Dimetridazole 142.1 96.1, 81.1 16, 28 [M+H]+ 4.72
49 Doramectin 921.5 777.4, 449.3 44, 56 [M+Na]+ 18.55
50 Doxycycline 445.2 428.1, 321.1 16, 28 [M+H]+ 8.30
51 Enoxacin 321.1 303.3, 231.8 16, 40 [M+H]+ 4.83
52 Enrofloxacin 360.2 316.2, 245.1 16, 32 [M+H]+ 5.84
53 Eprinomectin B1a 936.5 490.2, 352.1 56, 60 [M+Na]+ 17.42
54 Erythromycin 734.5 576.3, 158.1 16, 32 [M+H]+ 11.35
55 Ethopabate 238.1 205.9, 135.9 4, 36 [M+H]+ 9.80
56 Febantel 447.1 415.1, 383.1 10, 16 [M+H]+ 15.66
57 Fenbendazole 300.1 268.1, 159.0 20, 36 [M+H]+ 14.31
58 Fleroxacin 370.1 326.0, 268.9 20, 24 [M+H]+ 5.11
59 Florfenicol 356.0 185.1, 119.0 12, 28 [M-H]- 8.43
60 Flubendazole 314.1 282.1, 123.0 20, 36 [M+H]+ 13.08
61 Fludrocortisone acetate 423.2 239.0, 121.0 24, 40 [M+H]+ 14.05
62 Flumequine 262.1 244.1, 202.0 12, 32 [M+H]+ 12.90
63 Flumethasone 411.2 391.1, 253.1 4, 12 [M+H]+ 13.04
64 Halofuginone 416.0 138.0, 395.8 16, 12 [M+H]+ 8.53
65 Haloperidol 376.1 165.0, 122.9 24, 48 [M+H]+ 11.83
66 Hydroxydimetridazole 158.1 140.0, 55.2 8, 20 [M+H]+ 3.95
67 Hydrocortisone 363.4 121.1, 309.2 20, 20 [M+H]+ 10.69
68 Hydroxymetronidazole 188.1 126.1, 123.1 16, 8 [M+H]+ 3.52
69 Hydroxy-thiabendazole 218.0 191.0, 147.1 32, 40 [M+H]+ 3.93
70 Indomethacin 358.1 138.9, 110.9 24, 68 [M+H]+ 15.47
71 Indoprofen 282.1 236.1, 77.1 20, 76 [M+H]+ 13.57
72 Ivermectin B1a 897.5 753.4, 183.0 52, 56 [M+Na]+ 19.52
73 Kitasamycin 772.5 174.0, 108.9 36, 48 [M+H]+ 13.43
74 Leucomalachite green 331.2 316.2, 239.2 20, 28 [M+H]+ 16.95
75 Levamisole 205.1 178.1, 91.1 20, 44 [M+H]+ 4.48
76 Lincomycin 407.2 126.1, 42.2 29, 75 [M+H]+ 4.25
77 Lomefloxacin 352.2 308.2, 265.0 16, 25 [M+H]+ 5.56
78 Maduramicin 939.5 895.6, 877.5 56, 36 [M+Na]+ 21.81
79 Marbofloxacin 363.2 320.1, 72.2 12, 28 [M+H]+ 4.82
80 Mebendazole 296.1 264.1, 77.0 20, 48 [M+H]+ 12.03
81 Mebendazole-amine 238.1 105.1, 77.1 28, 40 [M+H]+ 7.35
82 Mefenamic acid 242.1 224.1, 209.1 8, 28 [M+H]+ 16.03
83 Megestrol acetate 385.2 325.2, 267.2 8, 12 [M+H]+ 16.05
84 Melengestrol acetate 397.2 337.1, 279.0 12, 20 [M+H]+ 16.19
85 Meloxicam 352.0 140.9, 115.0 16, 16 [M+H]+ 14.58
86 Methaqualone 251.1 132.1, 91.0 37, 49 [M+H]+ 13.84
87 Methylprednisolone 375.2 357.2, 161.1 4, 16 [M+H]+ 12.53
88 Methyltestosterone 303.2 109.1, 97.1 32, 32 [M+H]+ 14.91
89 Metronidazole 172.1 128.0, 82.1 12, 24 [M+H]+ 3.99
90 Monensin 693.5 675.3, 461.3 40, 60 [M+H]+ 20.87
91 N-Acetyl dapson 291.1 197.9, 155.8 12, 16 [M+H]+ 8.12
92 Nalidixic acid 233.1 215.1, 159.1 20, 40 [M+H]+ 12.12
93 Nandrolone phenylpropionate 407.3 257.2, 105.1 18, 36 [M+H]+ 17.61
94 Nequinate 366.2 334.1, 91.0 16, 44 [M+H]+ 15.23
95 Nicarbazine 301.1 137.0, 106.9 20, 45 [M-H]- 15.12
96 Nigericin 742.5 125.0, 107.0 60, 70 [M+NH4]+ 20.32
97 Nitroxynil 288.9 162.0, 127.0 20, 28 [M-H]- 12.80
98 Norfloxacin 320.1 302.1, 231.1 25, 40 [M+H]+ 5.03
99 Ofloxacin 362.2 318.2, 261.1 20, 40 [M+H]+ 5.08
100 Olaquindox 264.1 143.0, 102.0 40, 56 [M+H]+ 3.58
101 Oleandomycin 688.3 544.3, 158.2 15, 25 [M+H]+ 10.36
102 Orbifloxacin 396.2 352.1, 295.1 16, 28 [M+H]+ 6.11
103 Oxacillin 402.0 243.0, 160.0 8, 8 [M+H]+ 13.50
104 Oxfendazole 316.1 284.0, 159.0 16, 32 [M+H]+ 8.62
105 Oxfendazole sulfone 332.1 300.1, 159.0 20, 40 [M+H]+ 11.18
106 Oxibendazole 250.1 218.1, 176.1 16, 28 [M+H]+ 8.94
107 Oxolinic acid 262.1 243.9, 159.9 20, 45 [M+H]+ 9.17
108 Oxytetracycline 461.2 426.1, 201.1 14, 48 [M+H]+ 5.18
109 Pefloxacin 334.2 290.1, 233.1 16, 28 [M+H]+ 5.17
110 Penbutolol 292.2 236.0, 133.0 12, 24 [M+H]+ 13.58
111 Penicilline G 335.1 176.0, 160.1 8, 8 [M+H]+ 11.09
112 Penicilline V 351.1 159.9, 113.9 8, 40 [M+H]+ 12.77
113 Piperacillin 518.2 143.0, 114.9 20, 70 [M+H]+ 10.34
114 Piroxicam 332.1 95.0, 78.0 20, 76 [M+H]+ 13.31
115 Prednisolone 361.2 343.2, 147.1 4, 24 [M+H]+ 10.45
116 Prednisone 359.2 341.2, 147.1 10, 40 [M+H]+ 10.50
117 Progesterone 315.2 109.0, 97.0 28, 24 [M+H]+ 16.17
118 Propanolol 260.0 116.0, 56.0 16, 28 [M+H]+ 9.56
119 Propionylpromazine 341.2 86.1, 58.1 20, 56 [M+H]+ 13.51
120 Ractopamine 302.2 284.2, 164.1 8, 12 [M+H]+ 5.51
121 Robenidine 334.1 155.0, 111.0 16, 56 [M+H]+ 14.14
122 Ronidazole 201.1 140.1, 55.2 8, 25 [M+H]+ 4.39
123 Salbutamol 240.2 166.1, 77.2 4, 60 [M+H]+ 3.44
124 Sarafloxacin 386.1 368.1, 342.1 20, 20 [M+H]+ 6.73
125 Sparfloxacin 393.2 349.0, 292.1 20, 28 [M+H]+ 6.92
126 Sulbactam 232.0 140.1, 64.1 12, 44 [M-H]- 3.74
127 Sulfabenzamide 277.1 155.9, 92.0 12, 36 [M+H]+ 9.72
128 Sulfacetamide 215.0 156.0, 92.0 8, 20 [M+H]+ 4.17
129 Sulfachloropyridazine 285.0 156.0, 108.1 12, 24 [M+H]+ 7.60
130 Sulfaclozine 285.0 155.9, 108.1 20, 24 [M+H]+ 9.85
131 Sulfadiazine 251.1 108.1, 92.1 20, 28 [M+H]+ 4.53
132 Sulfadimethoxine 311.1 156.0, 92.1 16, 36 [M+H]+ 10.13
133 Sulfamethazine 279.1 186.1, 92.1 12, 38 [M+H]+ 6.16
134 Sulfadoxine 311.1 156.0, 92.1 16, 32 [M+H]+ 8.20
135 Sulfaguanidine 215.1 156.0, 108.0 12, 24 [M+H]+ 2.68
136 Sulfamerazine 265.1 156.0, 92.1 12, 28 [M+H]+ 5.37
137 Sulfameter 281.1 156.0, 92.0 20, 40 [M+H]+ 6.25
138 Sulfamethizole 271.0 156.0, 92.0 9, 29 [M+H]+ 6.07
139 Sulfamethoxazole 254.1 156.0, 92.1 12, 24 [M+H]+ 8.25
140 Sulfamethoxypyridazine 281.1 108.1, 92.1 28, 32 [M+H]+ 4.03
141 Sulfamonomethoxine 281.0 156.0, 126.0 10, 20 [M+H]+ 7.10
142 Sulfamoxole 268.1 155.9, 108.0 20, 20 [M+H]+ 5.67
143 Sulfaphenazole 315.1 158.1, 92.0 40, 40 [M+H]+ 10.48
144 Sulfapyridine 250.1 156.0, 92.0 17, 29 [M+H]+ 5.03
145 Sulfaquinoxaline 301.1 156.0, 92.0 16, 32 [M+H]+ 10.19
146 Sulfathiazole 256.0 156.0, 92.1 12, 28 [M+H]+ 4.74
147 Sulfisomidine 279.1 124.1, 92.0 20, 40 [M+H]+ 4.03
148 Sulindac 357.1 248.1, 233.1 40, 40 [M+H]+ 13.67
149 Sulphisoxazole 268.1 156.0, 92.0 10, 40 [M+H]+ 8.81
150 Tenoxicam 338.0 121.0, 78.0 24, 72 [M+H]+ 8.73
151 Terbutaline 226.1 152.1, 107.1 12, 28 [M+H]+ 3.42
152 Testosterone 289.2 109.0, 97.0 32, 36 [M+H]+ 14.51
153 Testosterone propionate 345.2 109.0, 97.1 36, 20 [M+H]+ 17.24
154 Tetracycline 445.2 410.1, 154.2 17, 30 [M+H]+ 5.79
155 Thiabendazole 202.0 175.0, 131.0 24, 36 [M+H]+ 4.74
156 Thiamphenicol 354.0 289.9, 185.0 8, 16 [M-H]- 5.68
157 Tolfenamic acid 262.1 244.0, 209.1 12, 28 [M+H]+ 16.20
158 Tolmetin 258.1 119.0, 91.0 24, 44 [M+H]+ 14.09
159 Trenbolone 271.2 253.2, 199.1 20, 28 [M+H]+ 13.57
160 Triamcinolone 395.2 375.0, 357.2 8, 12 [M+H]+ 8.47
161 Triamcinolone acetonide 435.2 415.2, 397.1 8, 16 [M+H]+ 13.57
162 Triclabendazole 361.0 345.9, 274.0 28, 40 [M+H]+ 16.05
163 Trimethoprim 291.2 261.1, 123.1 24, 24 [M+H]+ 4.92
164 Tulobuterol 228.1 154.0, 119.1 12, 32 [M+H]+ 6.66
165 Tylosin 916.5 174.1, 101.0 40, 56 [M+H]+ 12.47
166 Tylvalosin 1042.6 173.9, 109.1 45, 52 [M+H]+ 14.39
167 Valnemulin 567.4 264.2, 263.0 16, 16 [M+H]+ 13.65
168 Xylazine 221.1 90.0, 72.0 40, 40 [M+H]+ 6.60
169 Zoalene 224.0 181.1, 77.0 12, 24 [M-H]- 8.11
), ArticleFig(id=1220364172936794852, tenantId=1146029695717560320, journalId=1189982191388893191, articleId=1220364157635973314, language=CN, label=Table 2, caption=

MS parameters of the 169 veterinary drugs

, figureFileSmall=null, figureFileBig=null, tableContent=
No. Compound Precursor ion (m/z) Product ion (m/z) CE/V Ionization mode RT/min
1 2-Aminoflubendazole 256.1 123.0, 95.0 40, 40 [M+H]+ 8.04
2 3-Methyl-quinoxaline-2-carboxylic acid 189.1 145.0, 143.0 12, 16 [M+H]+ 5.38
3 4-Acetamido antipyrine 246.1 227.9, 83.0 12, 40 [M+H]+ 4.76
4 4-Formylamino antipyrine 232.1 104.0, 83.0 20, 20 [M+H]+ 4.79
5 5-Hydroxymebendazole 298.1 266.1, 79.1 25, 44 [M+H]+ 7.64
6 Acepromazine 327.2 86.1, 58.1 20, 48 [M+H]+ 11.74
7 Albendazole 266.1 234.1, 191.0 16, 32 [M+H]+ 12.75
8 Albendazole sulfone 298.1 266.1, 159.0 20, 40 [M+H]+ 8.50
9 Albendazole sulfoxide 282.1 239.9, 208.0 12, 24 [M+H]+ 6.31
10 Amantadine 152.1 135.0, 77.1 18, 50 [M+H]+ 5.18
11 Ampicillin 350.0 114.0, 106.0 36, 16 [M+H]+ 4.42
12 Avermectin B1a 895.5 751.4, 449.3 48, 48 [M+Na]+ 18.02
13 Azaperol 330.2 312.1, 121.0 16, 20 [M+H]+ 5.94
14 Azaperone 328.2 165.1, 121.1 20, 20 [M+H]+ 7.03
15 Basic violet 3 372.3 356.1, 340.0 44, 55 [M+H]+ 15.01
16 Betamethasone 393.2 373.2, 355.2 4, 8 [M+H]+ 13.01
17 Cambendazole 303.1 261.0, 217.1 16, 32 [M+H]+ 8.34
18 Carazolol 299.2 222.0, 116.0 20, 20 [M+H]+ 8.54
19 Carprofen 272.0 227.9, 225.9 12, 28 [M-H]- 15.16
20 Cefamandole 463.1 347.0, 158.0 4, 16 [M+H]+ 8.05
21 Cefapirin 424.1 291.9, 151.9 12, 28 [M+H]+ 3.74
22 Cefazolin 455.0 323.0, 156.0 8, 11 [M+H]+ 5.58
23 Cefetamet pivoxyl 512.1 241.0, 57.1 16, 48 [M+H]+ 14.23
24 Cefoperazone 646.2 530.2, 143.0 8, 45 [M+H]+ 7.21
25 Cefotaxime 456.1 324.0, 125.0 8, 60 [M+H]+ 5.11
26 Cefquinome 529.1 134.2, 125.0 8, 60 [M+H]+ 4.39
27 Ceftiofur 524.0 241.0, 126.0 16, 40 [M+H]+ 9.22
28 Cephalonium 459.1 337.0, 152.0 8, 20 [M+H]+ 4.82
29 Chloramphenicol 321.0 152.1, 121.0 14, 36 [M-H]- 9.19
30 Chlorpromazine 319.1 86.1, 58.2 16, 44 [M+H]+ 13.66
31 Chlortetracycline 479.1 444.0, 154.1 20, 36 [M+H]+ 7.95
32 Chlormadinone acetate 405.2 345.0, 309.0 12, 16 [M+H]+ 16.12
33 Cimaterol 220.1 202.1, 143.1 4, 20 [M+H]+ 3.57
34 Ciprofloxacin 332.1 314.0, 231.0 20, 48 [M+H]+ 5.23
35 Clenbuterol 277.1 259.1, 203.0 4, 12 [M+H]+ 6.75
36 Clopidol 192.1 101.0, 51.0 25, 48 [M+H]+ 4.23
37 Clorprenaline 214.1 196.0, 153.9 8, 12 [M+H]+ 5.62
38 Cloxacillin 436.0 277.0, 160.0 12, 12 [M+H]+ 14.00
39 Cortisone acetate 403.2 343.1, 163.0 20, 28 [M+H]+ 14.28
40 Danofloxacin 358.2 340.1, 82.1 20, 48 [M+H]+ 5.56
41 Dapson 249.1 156.0, 92.0 10, 28 [M+H]+ 7.25
42 Dexamethasone 393.2 373.2, 355.2 2, 6 [M+H]+ 12.88
43 Diazepam 285.1 193.1, 153.9 37, 29 [M+H]+ 14.91
44 Diclazuril 405.0 334.8, 334.0 16, 20 [M-H]- 15.58
45 Diclofenac 296.0 215.1, 214.1 16, 48 [M+H]+ 15.45
46 Dicloxacillin 470.0 310.8, 159.9 12, 12 [M+H]+ 14.53
47 Difloxacin 400.1 356.2, 299.1 16, 32 [M+H]+ 6.92
48 Dimetridazole 142.1 96.1, 81.1 16, 28 [M+H]+ 4.72
49 Doramectin 921.5 777.4, 449.3 44, 56 [M+Na]+ 18.55
50 Doxycycline 445.2 428.1, 321.1 16, 28 [M+H]+ 8.30
51 Enoxacin 321.1 303.3, 231.8 16, 40 [M+H]+ 4.83
52 Enrofloxacin 360.2 316.2, 245.1 16, 32 [M+H]+ 5.84
53 Eprinomectin B1a 936.5 490.2, 352.1 56, 60 [M+Na]+ 17.42
54 Erythromycin 734.5 576.3, 158.1 16, 32 [M+H]+ 11.35
55 Ethopabate 238.1 205.9, 135.9 4, 36 [M+H]+ 9.80
56 Febantel 447.1 415.1, 383.1 10, 16 [M+H]+ 15.66
57 Fenbendazole 300.1 268.1, 159.0 20, 36 [M+H]+ 14.31
58 Fleroxacin 370.1 326.0, 268.9 20, 24 [M+H]+ 5.11
59 Florfenicol 356.0 185.1, 119.0 12, 28 [M-H]- 8.43
60 Flubendazole 314.1 282.1, 123.0 20, 36 [M+H]+ 13.08
61 Fludrocortisone acetate 423.2 239.0, 121.0 24, 40 [M+H]+ 14.05
62 Flumequine 262.1 244.1, 202.0 12, 32 [M+H]+ 12.90
63 Flumethasone 411.2 391.1, 253.1 4, 12 [M+H]+ 13.04
64 Halofuginone 416.0 138.0, 395.8 16, 12 [M+H]+ 8.53
65 Haloperidol 376.1 165.0, 122.9 24, 48 [M+H]+ 11.83
66 Hydroxydimetridazole 158.1 140.0, 55.2 8, 20 [M+H]+ 3.95
67 Hydrocortisone 363.4 121.1, 309.2 20, 20 [M+H]+ 10.69
68 Hydroxymetronidazole 188.1 126.1, 123.1 16, 8 [M+H]+ 3.52
69 Hydroxy-thiabendazole 218.0 191.0, 147.1 32, 40 [M+H]+ 3.93
70 Indomethacin 358.1 138.9, 110.9 24, 68 [M+H]+ 15.47
71 Indoprofen 282.1 236.1, 77.1 20, 76 [M+H]+ 13.57
72 Ivermectin B1a 897.5 753.4, 183.0 52, 56 [M+Na]+ 19.52
73 Kitasamycin 772.5 174.0, 108.9 36, 48 [M+H]+ 13.43
74 Leucomalachite green 331.2 316.2, 239.2 20, 28 [M+H]+ 16.95
75 Levamisole 205.1 178.1, 91.1 20, 44 [M+H]+ 4.48
76 Lincomycin 407.2 126.1, 42.2 29, 75 [M+H]+ 4.25
77 Lomefloxacin 352.2 308.2, 265.0 16, 25 [M+H]+ 5.56
78 Maduramicin 939.5 895.6, 877.5 56, 36 [M+Na]+ 21.81
79 Marbofloxacin 363.2 320.1, 72.2 12, 28 [M+H]+ 4.82
80 Mebendazole 296.1 264.1, 77.0 20, 48 [M+H]+ 12.03
81 Mebendazole-amine 238.1 105.1, 77.1 28, 40 [M+H]+ 7.35
82 Mefenamic acid 242.1 224.1, 209.1 8, 28 [M+H]+ 16.03
83 Megestrol acetate 385.2 325.2, 267.2 8, 12 [M+H]+ 16.05
84 Melengestrol acetate 397.2 337.1, 279.0 12, 20 [M+H]+ 16.19
85 Meloxicam 352.0 140.9, 115.0 16, 16 [M+H]+ 14.58
86 Methaqualone 251.1 132.1, 91.0 37, 49 [M+H]+ 13.84
87 Methylprednisolone 375.2 357.2, 161.1 4, 16 [M+H]+ 12.53
88 Methyltestosterone 303.2 109.1, 97.1 32, 32 [M+H]+ 14.91
89 Metronidazole 172.1 128.0, 82.1 12, 24 [M+H]+ 3.99
90 Monensin 693.5 675.3, 461.3 40, 60 [M+H]+ 20.87
91 N-Acetyl dapson 291.1 197.9, 155.8 12, 16 [M+H]+ 8.12
92 Nalidixic acid 233.1 215.1, 159.1 20, 40 [M+H]+ 12.12
93 Nandrolone phenylpropionate 407.3 257.2, 105.1 18, 36 [M+H]+ 17.61
94 Nequinate 366.2 334.1, 91.0 16, 44 [M+H]+ 15.23
95 Nicarbazine 301.1 137.0, 106.9 20, 45 [M-H]- 15.12
96 Nigericin 742.5 125.0, 107.0 60, 70 [M+NH4]+ 20.32
97 Nitroxynil 288.9 162.0, 127.0 20, 28 [M-H]- 12.80
98 Norfloxacin 320.1 302.1, 231.1 25, 40 [M+H]+ 5.03
99 Ofloxacin 362.2 318.2, 261.1 20, 40 [M+H]+ 5.08
100 Olaquindox 264.1 143.0, 102.0 40, 56 [M+H]+ 3.58
101 Oleandomycin 688.3 544.3, 158.2 15, 25 [M+H]+ 10.36
102 Orbifloxacin 396.2 352.1, 295.1 16, 28 [M+H]+ 6.11
103 Oxacillin 402.0 243.0, 160.0 8, 8 [M+H]+ 13.50
104 Oxfendazole 316.1 284.0, 159.0 16, 32 [M+H]+ 8.62
105 Oxfendazole sulfone 332.1 300.1, 159.0 20, 40 [M+H]+ 11.18
106 Oxibendazole 250.1 218.1, 176.1 16, 28 [M+H]+ 8.94
107 Oxolinic acid 262.1 243.9, 159.9 20, 45 [M+H]+ 9.17
108 Oxytetracycline 461.2 426.1, 201.1 14, 48 [M+H]+ 5.18
109 Pefloxacin 334.2 290.1, 233.1 16, 28 [M+H]+ 5.17
110 Penbutolol 292.2 236.0, 133.0 12, 24 [M+H]+ 13.58
111 Penicilline G 335.1 176.0, 160.1 8, 8 [M+H]+ 11.09
112 Penicilline V 351.1 159.9, 113.9 8, 40 [M+H]+ 12.77
113 Piperacillin 518.2 143.0, 114.9 20, 70 [M+H]+ 10.34
114 Piroxicam 332.1 95.0, 78.0 20, 76 [M+H]+ 13.31
115 Prednisolone 361.2 343.2, 147.1 4, 24 [M+H]+ 10.45
116 Prednisone 359.2 341.2, 147.1 10, 40 [M+H]+ 10.50
117 Progesterone 315.2 109.0, 97.0 28, 24 [M+H]+ 16.17
118 Propanolol 260.0 116.0, 56.0 16, 28 [M+H]+ 9.56
119 Propionylpromazine 341.2 86.1, 58.1 20, 56 [M+H]+ 13.51
120 Ractopamine 302.2 284.2, 164.1 8, 12 [M+H]+ 5.51
121 Robenidine 334.1 155.0, 111.0 16, 56 [M+H]+ 14.14
122 Ronidazole 201.1 140.1, 55.2 8, 25 [M+H]+ 4.39
123 Salbutamol 240.2 166.1, 77.2 4, 60 [M+H]+ 3.44
124 Sarafloxacin 386.1 368.1, 342.1 20, 20 [M+H]+ 6.73
125 Sparfloxacin 393.2 349.0, 292.1 20, 28 [M+H]+ 6.92
126 Sulbactam 232.0 140.1, 64.1 12, 44 [M-H]- 3.74
127 Sulfabenzamide 277.1 155.9, 92.0 12, 36 [M+H]+ 9.72
128 Sulfacetamide 215.0 156.0, 92.0 8, 20 [M+H]+ 4.17
129 Sulfachloropyridazine 285.0 156.0, 108.1 12, 24 [M+H]+ 7.60
130 Sulfaclozine 285.0 155.9, 108.1 20, 24 [M+H]+ 9.85
131 Sulfadiazine 251.1 108.1, 92.1 20, 28 [M+H]+ 4.53
132 Sulfadimethoxine 311.1 156.0, 92.1 16, 36 [M+H]+ 10.13
133 Sulfamethazine 279.1 186.1, 92.1 12, 38 [M+H]+ 6.16
134 Sulfadoxine 311.1 156.0, 92.1 16, 32 [M+H]+ 8.20
135 Sulfaguanidine 215.1 156.0, 108.0 12, 24 [M+H]+ 2.68
136 Sulfamerazine 265.1 156.0, 92.1 12, 28 [M+H]+ 5.37
137 Sulfameter 281.1 156.0, 92.0 20, 40 [M+H]+ 6.25
138 Sulfamethizole 271.0 156.0, 92.0 9, 29 [M+H]+ 6.07
139 Sulfamethoxazole 254.1 156.0, 92.1 12, 24 [M+H]+ 8.25
140 Sulfamethoxypyridazine 281.1 108.1, 92.1 28, 32 [M+H]+ 4.03
141 Sulfamonomethoxine 281.0 156.0, 126.0 10, 20 [M+H]+ 7.10
142 Sulfamoxole 268.1 155.9, 108.0 20, 20 [M+H]+ 5.67
143 Sulfaphenazole 315.1 158.1, 92.0 40, 40 [M+H]+ 10.48
144 Sulfapyridine 250.1 156.0, 92.0 17, 29 [M+H]+ 5.03
145 Sulfaquinoxaline 301.1 156.0, 92.0 16, 32 [M+H]+ 10.19
146 Sulfathiazole 256.0 156.0, 92.1 12, 28 [M+H]+ 4.74
147 Sulfisomidine 279.1 124.1, 92.0 20, 40 [M+H]+ 4.03
148 Sulindac 357.1 248.1, 233.1 40, 40 [M+H]+ 13.67
149 Sulphisoxazole 268.1 156.0, 92.0 10, 40 [M+H]+ 8.81
150 Tenoxicam 338.0 121.0, 78.0 24, 72 [M+H]+ 8.73
151 Terbutaline 226.1 152.1, 107.1 12, 28 [M+H]+ 3.42
152 Testosterone 289.2 109.0, 97.0 32, 36 [M+H]+ 14.51
153 Testosterone propionate 345.2 109.0, 97.1 36, 20 [M+H]+ 17.24
154 Tetracycline 445.2 410.1, 154.2 17, 30 [M+H]+ 5.79
155 Thiabendazole 202.0 175.0, 131.0 24, 36 [M+H]+ 4.74
156 Thiamphenicol 354.0 289.9, 185.0 8, 16 [M-H]- 5.68
157 Tolfenamic acid 262.1 244.0, 209.1 12, 28 [M+H]+ 16.20
158 Tolmetin 258.1 119.0, 91.0 24, 44 [M+H]+ 14.09
159 Trenbolone 271.2 253.2, 199.1 20, 28 [M+H]+ 13.57
160 Triamcinolone 395.2 375.0, 357.2 8, 12 [M+H]+ 8.47
161 Triamcinolone acetonide 435.2 415.2, 397.1 8, 16 [M+H]+ 13.57
162 Triclabendazole 361.0 345.9, 274.0 28, 40 [M+H]+ 16.05
163 Trimethoprim 291.2 261.1, 123.1 24, 24 [M+H]+ 4.92
164 Tulobuterol 228.1 154.0, 119.1 12, 32 [M+H]+ 6.66
165 Tylosin 916.5 174.1, 101.0 40, 56 [M+H]+ 12.47
166 Tylvalosin 1042.6 173.9, 109.1 45, 52 [M+H]+ 14.39
167 Valnemulin 567.4 264.2, 263.0 16, 16 [M+H]+ 13.65
168 Xylazine 221.1 90.0, 72.0 40, 40 [M+H]+ 6.60
169 Zoalene 224.0 181.1, 77.0 12, 24 [M-H]- 8.11
), ArticleFig(id=1220364173050041066, tenantId=1146029695717560320, journalId=1189982191388893191, articleId=1220364157635973314, language=EN, label=null, caption=null, figureFileSmall=null, figureFileBig=null, tableContent=
Supplier Result
Medicinal
material base
Ofloxacin, 3-methyl-quinoxaline-2-carboxylic acid
Albendazole sulfoxide
Ofloxacin
Ofloxacin
Ofloxacin
4-Acetamido antipyrine, ofloxacin
Ofloxacin
Ofloxacin
4-Acetamido antipyrine, 4-formylamino antipyrine, ofloxacin, diclofenac
Metronidazole, 4-acetamido antipyrine, 4-formylamino antipyrine, ofloxacin, enrofloxacin
Ofloxacin
Ivermectin
4-Acetamido antipyrine, 4-formylamino antipyrine, ivermectin
Open market Hydroxymetronidazole, metronidazole, lincomycin, albendazole sulfoxide, albendazole sulfone
Olaquindox, 4-acetamido antipyrine, 4-formylamino antipyrine, 3-methyl-quinoxaline-2-carboxylic acid, albendazole
sulfoxide, albendazole
Sulfamethoxypyridazine, 4-acetamido antipyrine, 4-formylamino antipyrine, trimethoprim, 3-methyl-quinoxaline-2-
carboxylic acid, sulfameter, sulfamonomethoxine, diclofenac, monensin
Hydroxymetronidazole, metronidazole, 4-acetamido antipyrine, 4-formylamino antipyrine, 3-methyl-quinoxaline-2-
carboxylic acid
), ArticleFig(id=1220364173180064492, tenantId=1146029695717560320, journalId=1189982191388893191, articleId=1220364157635973314, language=CN, label=Table 3, caption=

The detection results of positive results

, figureFileSmall=null, figureFileBig=null, tableContent=
Supplier Result
Medicinal
material base
Ofloxacin, 3-methyl-quinoxaline-2-carboxylic acid
Albendazole sulfoxide
Ofloxacin
Ofloxacin
Ofloxacin
4-Acetamido antipyrine, ofloxacin
Ofloxacin
Ofloxacin
4-Acetamido antipyrine, 4-formylamino antipyrine, ofloxacin, diclofenac
Metronidazole, 4-acetamido antipyrine, 4-formylamino antipyrine, ofloxacin, enrofloxacin
Ofloxacin
Ivermectin
4-Acetamido antipyrine, 4-formylamino antipyrine, ivermectin
Open market Hydroxymetronidazole, metronidazole, lincomycin, albendazole sulfoxide, albendazole sulfone
Olaquindox, 4-acetamido antipyrine, 4-formylamino antipyrine, 3-methyl-quinoxaline-2-carboxylic acid, albendazole
sulfoxide, albendazole
Sulfamethoxypyridazine, 4-acetamido antipyrine, 4-formylamino antipyrine, trimethoprim, 3-methyl-quinoxaline-2-
carboxylic acid, sulfameter, sulfamonomethoxine, diclofenac, monensin
Hydroxymetronidazole, metronidazole, 4-acetamido antipyrine, 4-formylamino antipyrine, 3-methyl-quinoxaline-2-
carboxylic acid
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QuEChERS-超高效液相色谱串联质谱法定性筛查中药材熊胆粉中169种兽药残留
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孙健 , 胡青 , 诸艳蓉 , 张甦 , 于泓 , 冯睿 , 张静娴 , 毛秀红 , 季申 *
药学学报 | 研究论文 2020,55(1): 113-122
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药学学报 | 研究论文 2020, 55(1): 113-122
QuEChERS-超高效液相色谱串联质谱法定性筛查中药材熊胆粉中169种兽药残留
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孙健, 胡青, 诸艳蓉, 张甦, 于泓, 冯睿, 张静娴, 毛秀红, 季申*
作者信息
  • 上海市食品药品检验所, 国家药品监督管理局中药质量控制重点实验室, 上海 201203

通讯作者:

*季申, Tel:86-21-50798195, E-mail:
Qualitative screening of 169 veterinary drug residues in bear bile powder by QuEChERS-ultra high performance liquid chromatography-tandem mass spectrometry
Jian SUN, Qing HU, Yan-rong ZHU, Su ZHANG, Hong YU, Rui FENG, Jing-xian ZHANG, Xiu-hong MAO, Shen JI*
Affiliations
  • NMPA Key Laboratory for Quality Control of Traditional Chinese Medicine, Shanghai Institute for Food and Drug Control, Shanghai 201203, China
出版时间: 2020-01-12 doi: 10.16438/j.0513-4870.2019-0531
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建立了QuEChERS-超高效液相色谱串联质谱法定性筛查中药材熊胆粉中多种兽药残留,包括β-受体激动剂与拮抗剂、抗生素(青霉素类、头孢菌素类、磺胺类、喹诺酮类、氯霉素类、四环素类、硝基咪唑类、大环内酯类、聚醚类等)、抗病毒药、驱虫药、甾体激素、非甾体抗炎药和镇静剂等169种兽药残留。样品经Na2EDTA-McIlvaine缓冲液和5%甲酸乙腈提取,经分散固相萃取法净化,以超高效液相色谱串联三重四极杆质谱法测定,通过离子丰度比定性判定。169种化合物检出限为1~1 000 μg·kg-1。本方法简便快速,已应用于实际样品的测定,并可扩展至其他类似药材基质的检测。

QuEChERS  /  超高效液相色谱串联质谱  /  兽药  /  熊胆粉  /  定性筛查

A QuEChERS-ultra high performance liquid chromatography-tandem mass spectrometry method was developed for qualitative screening of 169 veterinary drug residues in bear bile powder, including β-agonists and inhibitors, antibiotics (penicillins, β-lactams, sulfomamides, quinolones, chloramphenicals, tetracyclines, nitroimidazoles, macrolides, polyethers, etc.), antiviral drugs, anthelminitics, steroid hormones, nonsteroidal antiinflammatory drugs (NSAIDs) and sedatives. The samples were extracted by Na2EDTA-McIlvaine buffer solution and 5% fomic acid-acetonitrile solution, then purified by dispersive solid phase extraction. Detection of veterinary drug residues by ultra high performance liquid chromatography-triple quadrupole mass spectrometry was conducted and qualitative confirmed by ion ratios. The limits of detection of 169 veterinary drugs were 1-1 000 μg·kg-1. The method is simple and fast, which had been used for the analysis of actual samples, and can be extended to the detection of similar matrix.

QuEChERS  /  ultra high performance liquid chromatography-tandem mass spectrometry  /  veterinary drug  /  bear bile powder  /  qualitative screening
孙健, 胡青, 诸艳蓉, 张甦, 于泓, 冯睿, 张静娴, 毛秀红, 季申. QuEChERS-超高效液相色谱串联质谱法定性筛查中药材熊胆粉中169种兽药残留. 药学学报, 2020 , 55 (1) : 113 -122 . DOI: 10.16438/j.0513-4870.2019-0531
Jian SUN, Qing HU, Yan-rong ZHU, Su ZHANG, Hong YU, Rui FENG, Jing-xian ZHANG, Xiu-hong MAO, Shen JI. Qualitative screening of 169 veterinary drug residues in bear bile powder by QuEChERS-ultra high performance liquid chromatography-tandem mass spectrometry[J]. Acta Pharmaceutica Sinica, 2020 , 55 (1) : 113 -122 . DOI: 10.16438/j.0513-4870.2019-0531
兽药广泛用于动物养殖过程中, 规范使用兽药可有效减少动物病患, 但若违规超量超范围使用兽药, 将对食品药品安全带来风险。目前, 动物源性食品中兽药残留带来的安全风险已成为共识, 政府及社会给予的重视程度较高。但动物源性中药材, 在动物养殖过程中滥用兽药的情况同样存在, 针对此类基质的检测方法研究及限量规定目前仍为空白, 急需引起关注和加深研究, 从源头进行有效控制。
熊胆粉为熊胆汁的干燥品。在黑熊胆囊手术引流胆汁过程中, 需使用塞拉嗪等镇静剂、青霉素等抗生素; 术后恢复过程使用氧氟沙星等抗生素。另外, 对某基地的黑熊喂养饲料进行检测, 检出土霉素、四环素、喹乙醇等兽药。因此有必要对熊胆粉的多种兽药残留进行监控。
针对动物源性食品的兽药残留检测研究较多, 相关国标(GB/T 22338-2008、GB/T 21317-2007、GB/T 21312-2007等)多按化合物类别分别检测; 文献[1-8]方法大多研究多种兽药残留的快速测定方法。文献报道的食品中兽药残留检测的前处理方法有液液萃取法[1]、载体辅助液液萃取法[2]、固相萃取法[3, 4]、QuEChERS法[5, 6]等, 检测技术有高效液相色谱法[7]、高效液相色谱串联三重四极杆质谱法[5, 6]、高效液相色谱串联四极杆飞行时间质谱法[8]、高效液相色谱串联三重四极杆线性离子阱质谱法[9]、高效液相色谱串联四极杆静电场轨道阱质谱法[10]等。
动物类中药材基质复杂, 多为干物质, 药效成分多, 不易净化, 较食品检测更为困难。本文研究对象熊胆粉, 牛磺熊去氧胆酸和牛磺鹅去氧胆酸等胆汁酸占44%~61%[11], 与多数弱酸性小分子药物化学结构有相似性, 因去除困难而对检测带来较强干扰; 其他成分还包括胆红素、蛋白质、氨基酸和微量元素等, 是基质非常复杂特殊的动物类中药材。因此需根据中药材的特殊性质, 针对性地研究开发与食品不同的前处理方法和检测条件。
根据农业部235号公告[12]及相关国标, 结合市场调研以及实际样品中的检测情况, 本文采用QuEChERS法对熊胆粉样品进行前处理, 以超高效液相色谱串联三重四极杆质谱法定性测定熊胆粉药材中的兽药残留共检测169种兽药, 主要包括: β-受体激动剂与拮抗剂、抗生素(青霉素类、头孢菌素类、磺胺类、喹诺酮类、氯霉素类、四环素类、硝基咪唑类、大环内酯类、聚醚类等)、抗病毒药、驱虫药(苯并咪唑类等)、甾体激素、非甾体抗炎药和镇静剂。
仪器与试剂  Agilent 1290/6495超高效液相色谱串联三重四极杆质谱仪(美国Agilent公司), N-EVAPTM 112型氮吹仪(美国Organomation公司); IKA KS260C振荡器和IKA MS 2涡旋混合器(德国IKA公司)。
兽药对照品:青霉素G采购自中国食品药品检定研究院, 其余167种购自A Chemtek公司, 见表 1; 乙腈、甲醇、乙酸均为色谱纯(美国MERCK公司); 醋酸, 分析纯(中国医药集团上海化学试剂公司); 甲酸、甲酸铵、氟化铵, 色谱纯(美国Sigma-Aldrich公司); 吸附剂: N-丙基乙二胺(PSA)、石墨化炭黑(GCB)、十八烷基键合硅胶(C18)、硫酸镁均购于天津博纳艾杰尔科技有限公司。实际样品由上海凯宝药业股份有限公司购自其熊胆粉药材供货商。
色谱和质谱条件   Agilent Zorbax Eclipse plus C18 (3.0 mm×150 mm, 1.8 μm)为色谱柱, 以0.2%甲酸(含5 mmol·L-1甲酸铵和0.5 mmol·L-1氟化铵)溶液为流动相A, 以0.2%甲酸乙腈溶液为流动相B, 梯度洗脱程序: 0~0.5 min, 2% B; 0.5~1.8 min, 2% B~15% B; 1.8~3.5 min, 15% B~20% B; 3.5~6 min, 20% B~25% B; 6~7 min, 25% B~30% B; 7~11 min, 30% B~35% B; 11~16 min, 35% B~100% B; 16~26 min, 100% B。柱温40 ℃, 流速0.5 mL·min-1, 进样量1 μL。
离子源:电喷雾离子(ESI)源; 离子源温度: 200 ℃; 毛细管电压: 4 kV; 干燥气流量: 12 L·min-1; 雾化气压力: 25 psi (1 psi≈6.9 kPa); 鞘气温度: 250 ℃; 鞘气流量: 10 L·min-1; 喷嘴电压: 500 V; 采用多反应监测(MRM)方式检测。各化合物质谱参数见表 2
标准溶液制备方法  对照品储备溶液(100 μg·mL-1):精密称取各对照品适量, 根据溶解性, 加适宜溶剂(表 1)制成每1 mL含100 μg的溶液, 即得。
混合对照品溶液(1 μg·mL-1):精密量取对照品储备溶液(100 μg·mL-1)适量, 用15%乙腈制成每mL含1 μg的溶液, 即得。
基质混合对照品溶液的制备:取空白熊胆粉样品(未检出上述169种兽药残留)适量, 研细, 混匀, 取约0.1 g, 精密称定, 置于50 mL聚苯乙烯具塞离心管中, 精密加入混合对照品溶液(1 μg·mL-1) 100 μL, 同供试品溶液的制备方法处理, 即得。
供试品溶液制备方法  取熊胆粉样品适量, 研细, 混匀, 取约0.1 g, 精密称定, 置于50 mL聚苯乙烯具塞离心管中, 加0.1 mol·L-1 Na2EDTA-McIlvaine缓冲液(称取2.9 g柠檬酸一水合物、10.9 g磷酸氢二钠十二水合物、37.2 g乙二胺四乙酸二钠二水合物, 加水至900 mL, 用1 mol·L-1氢氧化钠溶液调至pH 4.0, 用水定容至1 L) 10 mL, 摇匀, 涡旋使充分浸润。精密加入5%冰醋酸乙腈10 mL, 涡旋使混匀, 置振荡器上剧烈振荡(500次·min-1) 10 min。加入无水氯化钠-硫酸钠(1:4)混合粉末5 g, 再置振荡器上剧烈振荡(500次·min-1) 3 min, 离心5 min, 使分层。吸取上清液6 mL, 置已预先装有净化材料的分散固相萃取净化管[硫酸镁300 mg, 十八烷基硅烷键合硅胶300 mg, N-丙基乙二胺(PSA) 1 800 mg]中, 涡旋使充分混匀, 再置振荡器上剧烈振荡(500次·min-1) 5 min使净化完全, 离心5 min, 精密吸取上清液2 mL, 置氮吹仪上于40 ℃水浴浓缩至干, 精密加0.2 mL 15%乙腈, 涡旋1 min, 超声1 min, 混匀, 离心, 取上清液, 即得。
定性判定方法  供试品溶液若检出与对照品保留时间相同的色谱峰, 且所选择的离子丰度比与对照品溶液的离子丰度比一致(相对比例 > 50%, 允许±20%偏差; 相对比例20%~50%, 允许±25%偏差; 相对比例10%~20%, 允许±30%偏差; 相对比例 < 10%, 允许±50%偏差), 可判定具有该成分。
专属性  取空白样品适量, 同供试品溶液的制备方法处理, 进样测定。
检出限  取熊胆粉空白样品适量, 研细, 混匀, 取约0.1 g, 一式7份, 精密称定, 置于50 mL聚苯乙烯具塞离心管中, 分别精密加入混合对照品溶液(100 ng·mL-1) 1、10、50、100、250、500和1 000 μL, 同供试品溶液的制备方法处理, 进样测定。采用目视评价法, 以真实最低检出浓度作为检出限。
重复性  在加样(1 000 μg·kg-1)水平进行重复性实验, 一式6份, 进样测定。
空白样品未检出上述兽药残留, 表明空白基质对测定无干扰。
上述169种化合物检出限为1~1 000 μg·kg-1, 详见表 1。熊胆粉由熊胆汁干燥而得, 产率约10%。按农业部235号公告暂定熊胆汁中兽药残留限量, 并以产率折算至熊胆汁中, 本方法检出限能够满足定性筛查的需要。
在加样(1 000 μg·kg-1)水平进行重复性实验, 一式6份, 均检出上述兽药。各化合物MRM色谱图见图 1
检测44批熊胆粉样品, 其中17批检出, 检出率38.6%, 共检出19种兽药残留, 具体情况见表 3
其中, 由药材基地提供规范养殖的40批样品, 13批检出, 检出兽药种类少, 主要包括氧氟沙星、3-甲基喹噁啉-2-羧酸(喹乙醇代谢物)、阿苯达唑亚砜(阿苯达唑代谢物)、4-乙酰胺基安替比林(安替比林代谢物), 含量均较低。推测氧氟沙星为黑熊术后恢复用药, 喹乙醇为饲料带入。而购自市场的4批劣质药材, 均检出多种兽药残留, 且含量很高。可见中药材规范养殖或种植的必要性。
目前, 多兽药残留同时测定的前处理方法主要包括EMR-Lipid固相萃取法和QuEChERS法。但EMR-Lipid固相萃取法对长链结构物质具较强吸附力, 能有效降低肉类等高脂肪食品的基质干扰[13], 但不适用于熊胆粉此类的以小分子成分占多数的中药材。
以能代表各类别结构类型的15种化合物作为指标, 考察优化QuEChERS法各步骤。①提取水相:考察NaOH溶液、Na2EDTA-McIlvaine缓冲液和1%醋酸溶液, 结果表明必须使用Na2EDTA-McIlvaine缓冲液方能将四环素类从水层提取出来; ②提取有机相:考察乙腈、5%醋酸乙腈溶液和15%醋酸乙腈溶液的提取效率, 结果表明, 多数化合物使用5%醋酸乙腈溶液的峰面积稍高; ③净化材料:因熊胆粉基质中胆汁酸含量较高, 且成分复杂, 考察PSA、PAX (强阴离子交换)、GCB (石墨化炭)等多种吸附材料及其比例, 最终确定硫酸镁、C18、PSA (1:1:6)作为吸附材料, 可最大程度的吸附酸性基质, 降低基质效应。
于流动相水相(0.2%甲酸溶液)中加入5 mmol·L-1甲酸铵, 可缓冲熊胆粉基质的酸性, 减少样品中部分化合物保留时间与对照品的差异; 加入0.5 mmol·L-1氟化铵可极大优化四环素类化合物的峰形。因此流动相水相最终确定为0.2%甲酸(含5 mmol·L-1甲酸铵和0.5 mmol·L-1氟化铵)溶液。
综上, 本研究采用QuEChERS前处理方法, 建立了超高效液相色谱串联质谱法定性筛查熊胆粉中169种兽药残留。本文方法为其他动物药材提供了借鉴思路。可以该方法为基础, 结合具体基质的特点, 从提取方法、净化技术、色谱条件等多个方面进行研究和优化, 以尽可能去除干扰和基质效应, 将方法扩展应用至不同基质中。比如, 本研究团队调整了净化填料, 已成功建立了山羊角中173种兽药残留的定性筛查方法, 以及药用辅料炼蜜和含炼蜜的中成药中41种兽药残留的定性筛查方法。
由于基质的复杂性, 同时建立近两百种化合物的定量测定方法较为困难, 部分化合物回收率较低。未来将在定性筛查并初步定量的基础上, 进行安全风险评估, 针对安全风险较高的兽药品种(如熊胆粉中氧氟沙星、甲硝唑、安替比林和喹乙醇等)建立专属性定量检测方法, 并制定合理限度, 用标准倒逼源头养殖的规范化, 全面控制动物源性中药材的安全性风险。
  • 国家中药标准化项目(ZYBZH-C-SH-48)
  • 上海市科委技术平台项目(18DZ2292200)
  • 上海市科委技术标准专项(18DZ2200900)
  • 上海市科委课题(18395810300)
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2020年第55卷第1期
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doi: 10.16438/j.0513-4870.2019-0531
  • 接收时间:2019-07-05
  • 首发时间:2026-01-20
  • 出版时间:2020-01-12
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  • 收稿日期:2019-07-05
  • 修回日期:2019-08-21
基金
国家中药标准化项目(ZYBZH-C-SH-48)
上海市科委技术平台项目(18DZ2292200)
上海市科委技术标准专项(18DZ2200900)
上海市科委课题(18395810300)
作者信息
    上海市食品药品检验所, 国家药品监督管理局中药质量控制重点实验室, 上海 201203

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2种不同金属材料的力学参数

Family
属数
Number of
genus
种数
Number of
species
占总种数比例
Percentage of
total species (%)

Genus
种数
Number of
species
占总种数比例
Percentage of total
species (%)
鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
小菇科 Mycenaceae 2 12 5.74 丝盖伞属 Inocybe 5 2.39
多孔菌科 Polyporaceae 8 14 6.70 蜡蘑属 Laccaria 5 2.39
红菇科 Russulaceae 3 23 11.00 小皮伞属 Marasmius 6 2.87
小菇属 Mycena 11 5.26
光柄菇属 Pluteus 5 2.39
红菇属 Russula 17 8.13
栓菌属 Trametes 5 2.39
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