Article(id=1206272758095344024, tenantId=1146029695717560320, journalId=1205117023404326918, issueId=1206272755658453329, articleNumber=null, orderNo=null, doi=10.16155/j.0254-1793.2024-1214, pmid=null, cstr=null, oa=null, hot=1, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1729180800000, receivedDateStr=2024-10-18, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1765527436994, onlineDateStr=2025-12-12, pubDate=null, pubDateStr=null, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1765527436994, onlineIssueDateStr=2025-12-12, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1765527436994, creator=13701087609, updateTime=1773896873946, updator=13701087609, issue=Issue{id=1206272755658453329, tenantId=1146029695717560320, journalId=1205117023404326918, year='2025', volume='45', issue='5', pageStart='739', pageEnd='920', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=1, specialIssue=0, createTime=1765527436411, creator=13701087609, updateTime=1765531454840, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1206289610234196753, tenantId=1146029695717560320, journalId=1205117023404326918, issueId=1206272755658453329, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1206289610234196754, tenantId=1146029695717560320, journalId=1205117023404326918, issueId=1206272755658453329, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=889, endPage=900, ext={EN=ArticleExt(id=1206272758321836456, articleId=1206272758095344024, tenantId=1146029695717560320, journalId=1205117023404326918, language=EN, title=UPLC-QQQ MS/MS with solid phase extraction for simultaneous determination of 68 veterinary drug residues in Galli Gigerii Endothelium Corneum, columnId=1206272757852074373, journalTitle=Chinese Journal of Pharmaceutical Analysis, columnName=Safety Monitoring, runingTitle=null, highlight=null, articleAbstract=

Objective: To establish a method for the determination of veterinary drug residues in Galli Gigerii Endothelium Corneum by ultra high performance liquid chromatography-tandem triple quadrupole mass spectrometry (UPLC-QQQ MS/MS) with solid-phase extraction. Methods: The samples were evenly dispersed,extracted with acetonitrile and acetonitrile containing 0.5% formic acid, and cleaned up with Oasis PRiME HLB solid phase extraction columns. The extracts were separated on Agilent ZORBAX Eclipse Plus C18 (3.0 mm×150 mm, 1.8 μm) using 5 mmol · L-1 ammonium acetate and acetonitrile (containing 0.1% formic acid) as mobile phase by gradient elution. The detection of veterinary drug residues was detected by tandem mass spectrometry with positive electrospray ion source under multiple reaction monitoring (MRM) mode. The matrix-matched external standard method was used for the quantitation. Results: The method exhibited good linearities within a certain concentration range r≥0.995 8. The limits of detection (LODs) were in the range of 0.1-3 μg · kg-1. The limits of quantitation (LOQs) were in the range of 0.2-10 μg · kg-1. The good recovery values (61.9%-121.5%) were achieved for all the 68 veterinary drugs with RSDs ranging from 0.50% to 8.4% for spiking 3 different levels. Out of 50 batches of samples, 5 batches of Galli Gigerii Endothelium Corneum were found to contain veterinary drug residues,including amantadine, doxycycline, enrofloxacin, and florfenicol. Conclusion: This method proves suitable for the rapid determination of multiple veterinary drug residues in Galli Gigerii Endothelium Corneum, with a simple,quick, accurate and procedure.

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目的:建立固相萃取-超高效液相色谱串联三重四极杆质谱法(UPLC-QQQ MS/MS法)测定中药鸡内金中68种兽药残留。方法:样品匀质后,经乙腈和含0.5%甲酸的乙腈进行2次提取,并经Oasis PRiME HLB固相萃取柱净化。采用Agilent ZORBAX Eclipse Plus C18(3.0 mm×150 mm,1.8 μm)色谱柱分离,以乙腈和5 mmol · L-1乙酸铵水溶液(含0.1%甲酸)体系为流动相进行梯度洗脱;ESI电离源,正、负离子模式,多反应监测(MRM),空白基质匹配标准曲线法定量。结果:68种兽药在一定质量浓度范围内线性关系良好,r≥0.995 8;方法检测限(LOD)为0.1~3 μg · kg-1,定量限(LOQ)为0.2~10 μg · kg-1;3个浓度水平下(n=6)加样回收率在61.9%~121.5%,RSD为0.50%~8.4%。在50批鸡内金样品中共有5批检出兽药残留,检出的兽药残留包括金刚烷胺、多西环素、恩诺沙星、氟苯尼考。结论:本方法简便、快捷、准确、可靠,适用于鸡内金中多种兽药残留的测定。

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glufosinate,glyphosate and their metabolites in sediment by ultra-high performance liquid chromatography-tandem mass spectrometry with pass-through solid-phase extraction,[J].Chin J Chromatogr202543(2):155, articleTitle=Determination of glufosinate,glyphosate and their metabolites in sediment by ultra-high performance liquid chromatography-tandem mass spectrometry with pass-through solid-phase extraction,, refAbstract=null), Reference(id=1206300941070955379, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1206272758095344024, doi=null, pmid=null, pmcid=null, year=2018, volume=16, issue=6, pageStart=807, pageEnd=null, url=null, language=null, rfNumber=[22], rfOrder=32, authorNames=孙爱萍, 袁波, 杨玉军, journalName=中南药学, refType=null, unstructuredReference=孙爱萍,袁波,杨玉军,等.鸡内金炮制的现代研究进展[J].中南药学201816(6):807, articleTitle=鸡内金炮制的现代研究进展, refAbstract=null), Reference(id=1206300941154841461, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1206272758095344024, doi=null, pmid=null, pmcid=null, year=2018, volume=16, issue=6, pageStart=807, pageEnd=null, url=null, language=null, rfNumber=[22], rfOrder=33, authorNames=SUN AP, YUAN B, YANG YJ, journalName=Cent South Pharm, refType=null, unstructuredReference=SUN APYUAN BYANG YJet al.Advances in modern research on Corneum processing[J].Cent South Pharm201816(6):807, articleTitle=Advances in modern research on Corneum processing, refAbstract=null)], funds=[Fund(id=1206300936427860731, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1206272758095344024, awardId=CY2022227, language=CN, fundingSource=*浙江省市场监督管理局雏鹰计划核心项目(CY2022227), fundOrder=null, country=null), Fund(id=1206300936494969599, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1206272758095344024, awardId=ZN2021002, language=CN, fundingSource=温州市重大科技创新攻关项目(ZN2021002), fundOrder=null, country=null)], companyList=[AuthorCompany(id=1206300931315003980, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1206272758095344024, xref=null, ext=[AuthorCompanyExt(id=1206300931323392590, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1206272758095344024, companyId=1206300931315003980, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=Wenzhou Research Institute for Food and Drug Control, Wenzhou 325000, China), AuthorCompanyExt(id=1206300931331781200, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1206272758095344024, companyId=1206300931315003980, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=温州市食品药品检验科学研究院,温州 325000)])], figs=[ArticleFig(id=1206300934989214394, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1206272758095344024, language=EN, label=Fig. 1, caption=The effects of heating on veterinary drug residues, figureFileSmall=qqqsMs70fSzOKP/DZBFVkw==, figureFileBig=HsbE3zYaBBmmzTTnU7lVPQ==, tableContent=null), ArticleFig(id=1206300935094071997, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1206272758095344024, language=CN, label=图1, caption=加热对兽药残留的影响, figureFileSmall=qqqsMs70fSzOKP/DZBFVkw==, figureFileBig=HsbE3zYaBBmmzTTnU7lVPQ==, tableContent=null), ArticleFig(id=1206300935198929601, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1206272758095344024, language=EN, label=Tab. 1, caption=

The sample informations of Galli Gigerii Endothelium Corneum

, figureFileSmall=null, figureFileBig=null, tableContent=
样品编号
(sample No.)
质量标准
(quality standards)
炮制品
(processing product)
1~152020年版《中国药典》一部(ChP 2020. Vol Ⅰ)鸡内金(Galli Gigerii Endothelium Corneum)
16~252020年版《中国药典》一部(ChP 2020. Vol Ⅰ)炒鸡内金(fried Galli Gigerii Endothelium Corneum)
26~402015年版《浙江省中药炮制规范》(Zhejiang Province Standards of Processing Chinese Crud Drugs 2015 Edition)鸡内金(Galli Gigerii Endothelium Corneum)
41~502015年版《浙江省中药炮制规范》(Zhejiang Province Standards of Processing Chinese Crud Drugs 2015 Edition)炒鸡内金(gried Galli Gigerii Endothelium Corneum)
), ArticleFig(id=1206300935287009989, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1206272758095344024, language=CN, label=表1, caption=

鸡内金样品信息

, figureFileSmall=null, figureFileBig=null, tableContent=
样品编号
(sample No.)
质量标准
(quality standards)
炮制品
(processing product)
1~152020年版《中国药典》一部(ChP 2020. Vol Ⅰ)鸡内金(Galli Gigerii Endothelium Corneum)
16~252020年版《中国药典》一部(ChP 2020. Vol Ⅰ)炒鸡内金(fried Galli Gigerii Endothelium Corneum)
26~402015年版《浙江省中药炮制规范》(Zhejiang Province Standards of Processing Chinese Crud Drugs 2015 Edition)鸡内金(Galli Gigerii Endothelium Corneum)
41~502015年版《浙江省中药炮制规范》(Zhejiang Province Standards of Processing Chinese Crud Drugs 2015 Edition)炒鸡内金(gried Galli Gigerii Endothelium Corneum)
), ArticleFig(id=1206300935362507463, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1206272758095344024, language=EN, label=Tab. 2, caption=

Theacquisition parameters of 68 veterinary drugs by mass spectrometry paraments

, figureFileSmall=null, figureFileBig=null, tableContent=
序号
(No.)
化合物
(compond)
相对分子质量
(relative molecular mass)
母离子
(parent ion)
m/z
子离子
(daughter ion)
m/z
碰撞能量
(collision energy)/eV
保留时间
(retention time)/min
离子化模式
(ionization mode)
1金刚烷胺(amantadine)151.1152.1135.0*,77.120,525.23[M+H]+
2氯霉素(chloramphenicol)323.1321.0257.0*,152.112,329.50[M-H]-
3金霉素(chlortetracycline)478.1479.1444.0*,154.120,328.03[M+H]+
4西诺沙星(cinoxacin)262.1263.1245.0*,217.016,248.51[M+H]+
5环丙沙星(ciprofloxacin)331.1332.1314.0*,231.020,485.34[M+H]+
6克拉霉素(clarithromycin)747.5748.5158.0*,83.132,5613.71[M+H]+
7丹氟沙星(canofloxacin)357.2358.2340.1*,82.124,525.63[M+H]+
8双氟沙星(difloxacin)399.1400.1382.1*,299.124,327.02[M+H]+
9二甲硝咪唑(dimetridazole)141.1142.196.1*,81.116,285.23[M+H]+
104,4’-二硝基均二苯脲
(4,4’-dinitrocarbanilide)
302.2301.2137.0*,107.012,5215.28[M-H]-
11多西环素(doxycycline)444.2445.2428.1*,410.020,205.91[M+H]+
12依诺沙星(enoxacin)320.1321.1303.3*,231.820,404.95[M+H]+
13恩诺沙星(enrofloxacin)359.2360.2342.2*,316.224,205.94[M+H]+
14红霉素(erythromycin)733.5734.5576.3*,158.120,3211.38[M+H]+
15氟虫腈(fipronil)437.2435.1330.1*,250.140,2416.16[M-H]-
16氟甲腈(fipronil-desulfinyl)389.1387.1351.0*,282.136,1616.28[M-H]-
17氟虫腈亚砜fipronil-sulfide)421.2419.1383.2*,262.048,4416.48[M-H]-
18氟虫腈砜(fipronil-sulfone)453.2451.1282.1*,244.032,5616.44[M-H]-
19氟罗沙星(fleroxacin)369.1370.1326.0*,268.920,325.25[M+H]+
20氟苯尼考(florfenicol)358.2356.0356.0*,185.148,608.78[M-H]-
21氟苯尼考胺(florfenicol amine)247.3247.7230.0*,130.016,403.11[M+H]+
22氟甲喹(flumequine)261.1262.1244.1*,202.020,4013.22[M+H]+
23羟甲基甲硝咪唑(hydroxydimetridazole)157.1158.1140.0*,55.28,184.22[M+H]+
24羟基异丙硝唑(hydroxyipronidazole)185.2186.1168.0*,122.012,366.27[M+H]+
25羟基甲硝唑(hydroxymetronidazole)187.1188.1126.1*,123.116,83.76[M+H]+
26异丙硝唑(ipronidazole)169.2170.1124.1*,109.012,89.20[M+H]+
27林可霉素(lincomycin)406.2407.2359.2*,126.120,364.33[M+H]+
28洛美沙星(lomefloxacin)351.1352.2308.2*,265.016,285.51[M+H]+
29马波沙星(marbofloxacin)335.4363.2320.1*,72.216,284.84[M+H]+
30甲硝唑(metronidazole)171.1172.1128.1*,82.212,244.14[M+H]+
31诺氟沙星(norfloxacin)319.1320.1302.1*,231.124,485.00[M+H]+
32氧氟沙星(ofloxacin)361.1362.2318.2*,261.120,325.07[M+H]+
33奥比沙星(orbifloxacin)395.2396.2352.1*,295.120,286.07[M+H]+
34喹酸(oxolinic acid)261.1262.1244.0*,216.020,3212.79[M+H]+
35土霉素(oxytetracycline)460.2461.2443.2*,426.112,205.29[M+H]+
36培氟沙星(pefloxacin)333.2334.2290.1*,233.120,285.15[M+H]+
37金刚乙胺(rimantadine)179.2180.3163.2*,121.216,328.34[M+H]+
38罗红霉素(roxithromycin)836.5837.5679.4*,158.024,3613.74[M+H]+
39沙拉沙星(sarafloxacin)385.1386.1368.1*,342.124,206.59[M+H]+
40司帕沙星(sparfloxacin)392.2393.2349.0*,292.120,286.83[M+H]+
41苯甲酰磺胺(sulfabenzamide)276.1277.1155.9*,92.012,369.50[M+H]+
42磺胺醋酰(sulfacetamide)214.0215.0156.0*,92.012,282.89[M+H]+
43磺胺氯哒嗪(sulfachloropyridazine)284.0285.0156.0*,92.116,367.50[M+H]+
44磺胺嘧啶(sulfadiazine)250.1251.1108.1*,92.128,324.61[M+H]+
45磺胺二甲氧嘧啶(sulfadimethoxine)310.1311.1156.0*,92.120,408.21[M+H]+
46磺胺二甲基嘧啶(sulfadimidine)278.1279.1124.0*,92.128,404.14[M+H]+
47磺胺邻二甲氧嘧啶(sulfadoxine)310.1311.1156.0*,92.120,368.21[M+H]+
48磺胺脒(sulfaguanidine)214.1215.1156.0*,108.012,242.89[M+H]+
49磺胺甲基嘧啶(sulfamerazine)264.1265.1156.0*,92.116,325.48[M+H]+
50磺胺对甲氧嘧啶(sulfameter)280.3281.1215.1*,156.016,166.26[M+H]+
51磺胺甲噻二唑(sulfamethizole)270.0271.0156.0*,92.012,326.04[M+H]+
52磺胺甲基异唑(sulfamethoxazole)253.1254.1156.0*,92.116,288.12[M+H]+
53磺胺甲氧哒嗪(sulfamethoxypyridazine)253.1281.1108.1*,92.132,366.26[M+H]+
54磺胺间甲氧嘧啶(sulfamonomethoxine)280.1281.0156.0*,126.020,247.05[M+H]+
55磺胺唑(sulfamoxole)267.1268.1155.9*,108.016,285.77[M+H]+
56磺胺硝苯(sulfanitran)335.1336.1293.9*,156.08,813.11[M+H]+
57磺胺吡啶(sulfapyridine)249.1250.1156.0*,92.016,285.14[M+H]+
58磺胺苯吡唑(sulfaphenazole)314.4315.1158.1*,92.016,2810.31[M+H]+
59磺胺喹啉(sulfaquinoxaline)300.1301.1156.0*,92.016,3210.07[M+H]+
60磺胺噻唑(sulfathiazole)255.0256.0156.0*,92.116,324.77[M+H]+
61磺胺二甲异嘧啶(sulfisomidine)278.1279.1124.1*,92.024,364.14[M+H]+
62磺胺二甲异唑(sulphisoxazole)267.3268.1156.0*,92.016,365.77[M+H]+
63四环素(tetracycline)444.2445.2410.1*,154.220,325.74[M+H]+
64替米考星(tilmicosin)868.6869.6696.4*,174.148,489.43[M+H]+
65甲砜霉素(thiamphenicol)356.2354.0158.0*,290.020,445.94[M-H]-
66替硝唑(tinidazole)247.1248.1121.0*,82.124,525.66[M+H]+
67甲氧苄啶(trimethoprim)290.1291.2261.1*,123.128,284.93[M+H]+
68五氯酚(pentachlorophenol)266.3268.7288.7515.26[M-H]-
266.7266.75
264.7264.75
262.7262.7*5
), ArticleFig(id=1206300935446393546, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1206272758095344024, language=CN, label=表2, caption=

68种兽药的质谱采集参数

, figureFileSmall=null, figureFileBig=null, tableContent=
序号
(No.)
化合物
(compond)
相对分子质量
(relative molecular mass)
母离子
(parent ion)
m/z
子离子
(daughter ion)
m/z
碰撞能量
(collision energy)/eV
保留时间
(retention time)/min
离子化模式
(ionization mode)
1金刚烷胺(amantadine)151.1152.1135.0*,77.120,525.23[M+H]+
2氯霉素(chloramphenicol)323.1321.0257.0*,152.112,329.50[M-H]-
3金霉素(chlortetracycline)478.1479.1444.0*,154.120,328.03[M+H]+
4西诺沙星(cinoxacin)262.1263.1245.0*,217.016,248.51[M+H]+
5环丙沙星(ciprofloxacin)331.1332.1314.0*,231.020,485.34[M+H]+
6克拉霉素(clarithromycin)747.5748.5158.0*,83.132,5613.71[M+H]+
7丹氟沙星(canofloxacin)357.2358.2340.1*,82.124,525.63[M+H]+
8双氟沙星(difloxacin)399.1400.1382.1*,299.124,327.02[M+H]+
9二甲硝咪唑(dimetridazole)141.1142.196.1*,81.116,285.23[M+H]+
104,4’-二硝基均二苯脲
(4,4’-dinitrocarbanilide)
302.2301.2137.0*,107.012,5215.28[M-H]-
11多西环素(doxycycline)444.2445.2428.1*,410.020,205.91[M+H]+
12依诺沙星(enoxacin)320.1321.1303.3*,231.820,404.95[M+H]+
13恩诺沙星(enrofloxacin)359.2360.2342.2*,316.224,205.94[M+H]+
14红霉素(erythromycin)733.5734.5576.3*,158.120,3211.38[M+H]+
15氟虫腈(fipronil)437.2435.1330.1*,250.140,2416.16[M-H]-
16氟甲腈(fipronil-desulfinyl)389.1387.1351.0*,282.136,1616.28[M-H]-
17氟虫腈亚砜fipronil-sulfide)421.2419.1383.2*,262.048,4416.48[M-H]-
18氟虫腈砜(fipronil-sulfone)453.2451.1282.1*,244.032,5616.44[M-H]-
19氟罗沙星(fleroxacin)369.1370.1326.0*,268.920,325.25[M+H]+
20氟苯尼考(florfenicol)358.2356.0356.0*,185.148,608.78[M-H]-
21氟苯尼考胺(florfenicol amine)247.3247.7230.0*,130.016,403.11[M+H]+
22氟甲喹(flumequine)261.1262.1244.1*,202.020,4013.22[M+H]+
23羟甲基甲硝咪唑(hydroxydimetridazole)157.1158.1140.0*,55.28,184.22[M+H]+
24羟基异丙硝唑(hydroxyipronidazole)185.2186.1168.0*,122.012,366.27[M+H]+
25羟基甲硝唑(hydroxymetronidazole)187.1188.1126.1*,123.116,83.76[M+H]+
26异丙硝唑(ipronidazole)169.2170.1124.1*,109.012,89.20[M+H]+
27林可霉素(lincomycin)406.2407.2359.2*,126.120,364.33[M+H]+
28洛美沙星(lomefloxacin)351.1352.2308.2*,265.016,285.51[M+H]+
29马波沙星(marbofloxacin)335.4363.2320.1*,72.216,284.84[M+H]+
30甲硝唑(metronidazole)171.1172.1128.1*,82.212,244.14[M+H]+
31诺氟沙星(norfloxacin)319.1320.1302.1*,231.124,485.00[M+H]+
32氧氟沙星(ofloxacin)361.1362.2318.2*,261.120,325.07[M+H]+
33奥比沙星(orbifloxacin)395.2396.2352.1*,295.120,286.07[M+H]+
34喹酸(oxolinic acid)261.1262.1244.0*,216.020,3212.79[M+H]+
35土霉素(oxytetracycline)460.2461.2443.2*,426.112,205.29[M+H]+
36培氟沙星(pefloxacin)333.2334.2290.1*,233.120,285.15[M+H]+
37金刚乙胺(rimantadine)179.2180.3163.2*,121.216,328.34[M+H]+
38罗红霉素(roxithromycin)836.5837.5679.4*,158.024,3613.74[M+H]+
39沙拉沙星(sarafloxacin)385.1386.1368.1*,342.124,206.59[M+H]+
40司帕沙星(sparfloxacin)392.2393.2349.0*,292.120,286.83[M+H]+
41苯甲酰磺胺(sulfabenzamide)276.1277.1155.9*,92.012,369.50[M+H]+
42磺胺醋酰(sulfacetamide)214.0215.0156.0*,92.012,282.89[M+H]+
43磺胺氯哒嗪(sulfachloropyridazine)284.0285.0156.0*,92.116,367.50[M+H]+
44磺胺嘧啶(sulfadiazine)250.1251.1108.1*,92.128,324.61[M+H]+
45磺胺二甲氧嘧啶(sulfadimethoxine)310.1311.1156.0*,92.120,408.21[M+H]+
46磺胺二甲基嘧啶(sulfadimidine)278.1279.1124.0*,92.128,404.14[M+H]+
47磺胺邻二甲氧嘧啶(sulfadoxine)310.1311.1156.0*,92.120,368.21[M+H]+
48磺胺脒(sulfaguanidine)214.1215.1156.0*,108.012,242.89[M+H]+
49磺胺甲基嘧啶(sulfamerazine)264.1265.1156.0*,92.116,325.48[M+H]+
50磺胺对甲氧嘧啶(sulfameter)280.3281.1215.1*,156.016,166.26[M+H]+
51磺胺甲噻二唑(sulfamethizole)270.0271.0156.0*,92.012,326.04[M+H]+
52磺胺甲基异唑(sulfamethoxazole)253.1254.1156.0*,92.116,288.12[M+H]+
53磺胺甲氧哒嗪(sulfamethoxypyridazine)253.1281.1108.1*,92.132,366.26[M+H]+
54磺胺间甲氧嘧啶(sulfamonomethoxine)280.1281.0156.0*,126.020,247.05[M+H]+
55磺胺唑(sulfamoxole)267.1268.1155.9*,108.016,285.77[M+H]+
56磺胺硝苯(sulfanitran)335.1336.1293.9*,156.08,813.11[M+H]+
57磺胺吡啶(sulfapyridine)249.1250.1156.0*,92.016,285.14[M+H]+
58磺胺苯吡唑(sulfaphenazole)314.4315.1158.1*,92.016,2810.31[M+H]+
59磺胺喹啉(sulfaquinoxaline)300.1301.1156.0*,92.016,3210.07[M+H]+
60磺胺噻唑(sulfathiazole)255.0256.0156.0*,92.116,324.77[M+H]+
61磺胺二甲异嘧啶(sulfisomidine)278.1279.1124.1*,92.024,364.14[M+H]+
62磺胺二甲异唑(sulphisoxazole)267.3268.1156.0*,92.016,365.77[M+H]+
63四环素(tetracycline)444.2445.2410.1*,154.220,325.74[M+H]+
64替米考星(tilmicosin)868.6869.6696.4*,174.148,489.43[M+H]+
65甲砜霉素(thiamphenicol)356.2354.0158.0*,290.020,445.94[M-H]-
66替硝唑(tinidazole)247.1248.1121.0*,82.124,525.66[M+H]+
67甲氧苄啶(trimethoprim)290.1291.2261.1*,123.128,284.93[M+H]+
68五氯酚(pentachlorophenol)266.3268.7288.7515.26[M-H]-
266.7266.75
264.7264.75
262.7262.7*5
), ArticleFig(id=1206300935555445455, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1206272758095344024, language=EN, label=Tab. 3, caption=

The linear equations and correlation coefficients(r), limits of detection(LOD),limits of quantity (LOQ) and matrix effect

, figureFileSmall=null, figureFileBig=null, tableContent=
序号
(No.)
化合物
(compound)
线性方程
(linear equation)
rLOD/(ng · mL-1LOQ/(ng · mL-1基质效应
(matrix effect)/%
1金刚烷胺(amantadine)Y=1.081×105X+2.617×1040.999 90.20.5-8.7
2氯霉素(chloramphenicol)Y=1.093×103X+5.873×1020.998 20.20.5-14.6
3金霉素(chlortetracycline)Y=1.859×102X-4.225×1010.998 71516.8
4西诺沙星(cinoxacin)Y=1.080×105X-4.440×1040.998 90.20.5-42.2
5环丙沙星(ciprofloxacin)Y=1.670×104X+8.840×1030.999 30.31100.7
6克拉霉素(clarithromycin)Y=9.167×104X-3.971×1040.997 30.10.5-28.3
7丹氟沙星(canofloxacin)Y=6.002×104X-9.413×1030.999 50.3163.7
8双氟沙星(difloxacin)Y=3.505×104X-1.192×1040.999 60.41-3.9
9二甲硝咪唑(dimetridazole)Y=3.525×103X-2.211×1030.999 40.721.0
104,4’-二硝基均二苯脲
(4,4’-dinitrocarbanilide)
Y=1.171×104X-7.737×1020.999 60.10.5-13.2
11多西环素(doxycycline)Y=7.211×102X-1.790×1020.999 80.3117.7
12依诺沙星(enoxacin)Y=3.697×104X+9.790×1020.999 60.62108.5
13恩诺沙星(enrofloxacin)Y=6.618×104X-2.070×1040.999 60.31-6.8
14红霉素(erythromycin)Y=6.043×104X-3.631×1040.997 50.31-37.2
15氟虫腈(fipronil)Y=6.167×103X+3.109×1030.997 70.20.588.9
16氟甲腈(fipronil-desulfinyl)Y=2.348×104X-1.870×1030.999 70.20.59.0
17氟虫腈亚砜(fipronil-sulfide)Y=1.349×104X-3.591×1030.999 20.10.527.8
18氟虫腈砜(fipronil-sulfone)Y=1.383×104X-1.539×1030.999 70.20.5-4.6
19氟罗沙星(fleroxacin)Y=6.440×104X-5.630×1030.999 80.20.5-5.0
20氟苯尼考(florfenicol)Y=3.435×103X-1.217×1030.996 0310-7.3
21氟苯尼考胺(florfenicol amine)Y=5.787×103X+3.610×1030.996 10.20.55.2
22氟甲喹(flumequine)Y=1.649×105X-2.777×1040.998 30.41-17.4
23羟甲基甲硝咪唑(hydroxydimetridazole)Y=5.271×103X-2.453×1030.999 40.31-8.2
24羟基异丙硝唑(hydroxyipronidazole)Y=8.985×103X-4.000×1030.999 60.20.52.2
25羟基甲硝唑(hydroxymetronidazole)Y=8.474×102X+8.928×1010.997 40.20.5-49.9
26异丙硝唑(ipronidazole)Y=6.934×103X-2.813×1030.993 20.20.5-16.2
27林可霉素(lincomycin)Y=5.653×104X-4.586×1030.999 40.20.5-30.2
28洛美沙星(lomefloxacin)Y=3.706×105X-1.894×1030.999 90.41-1.5
29马波沙星(marbofloxacin)Y=8.297×104X-1.235×1040.999 40.314.6
30甲硝唑(metronidazole)Y=1.941×104X-1.081×1040.998 80.10.2-3.1
31诺氟沙星(norfloxacin)Y=1.409×104X+4.868×1030.999 50.31145.8
32氧氟沙星(ofloxacin)Y=8.826×104X-1.515×1040.999 30.3110.7
33奥比沙星(orbifloxacin)Y=6.713×104X-5.368×1030.999 30.20.5-14.7
34喹酸(oxolinic acid)Y=4.247×105X+9.243×1030.999 30.31-16.1
35土霉素(oxytetracycline)Y=3.259×102X-2.754×1020.999 70.7273.7
36培氟沙星(pefloxacin)Y=3.294×104X-5.310×1030.999 60.31-1.3
37金刚乙胺(rimantadine)Y=9.256×104X-5.884×1030.999 90.20.50.0
38罗红霉素(roxithromycin)Y=2.727×104X-1.180×1040.998 50.20.5-17.2
39沙拉沙星(sarafloxacin)Y=1.781×104X-3.932×1030.999 00.319.9
40司帕沙星(sparfloxacin)Y=6.255×104X-2.441×1040.999 70.31-10.7
41苯甲酰磺胺(sulfabenzamide)Y=9.860×103X-3.723×1030.999 90.20.5-2.5
42磺胺醋酰(sulfacetamide)Y=9.676×103X-2.522×1030.999 90.620.1
43磺胺氯哒嗪(sulfachloropyridazine)Y=4.746×103X-2.021×1030.999 80.20.511.4
44磺胺嘧啶(sulfadiazine)Y=9.565×103X-4.661×1030.999 90.20.511.2
45磺胺二甲氧嘧啶(sulfadimethoxine)Y=2.441×104X-1.383×1040.999 80.20.57.8
46磺胺二甲基嘧啶(sulfadimidine)Y=4.415×104X-1.646×1040.999 00.20.5-16.7
47磺胺邻二甲氧嘧啶(sulfadoxine)Y=1.315×104X-6.322×1030.999 70.20.5-0.7
48磺胺脒(sulfaguanidine)Y=8.070×103X-2.678×1030.999 80.20.51.5
49磺胺甲基嘧啶(sulfamerazine)Y=9.572×103X-3.500×1030.999 80.20.51.5
50磺胺对甲氧嘧啶(sulfameter)Y=1.969×104X-8.110×1030.999 70.20.525.8
51磺胺甲噻二唑(sulfamethizole)Y=6.058×103X-2.443×1030.999 60.20.51.5
52磺胺甲基异唑(sulfamethoxazole)Y=8.508×103X-4.536×1031.000 00.20.510.4
53磺胺甲氧哒嗪(sulfamethoxypyridazine)Y=1.055×103X-2.883×1020.999 10.72-15.1
54磺胺间甲氧嘧啶(sulfamonomethoxine)Y=4.919×103X-2.387×1030.999 90.20.53.9
55磺胺唑(sulfamoxole)Y=6.533×103X-2.688×1031.000 00.20.55.9
56磺胺硝苯(sulfanitran)Y=2.423×101X-5.3580.995 8210-25.8
57磺胺吡啶(sulfapyridine)Y=1.101×104X-9.653×1030.999 70.20.5-9.5
58磺胺苯吡唑(sulfaphenazole)Y=1.091×104X-3.947×1030.999 40.20.545.7
59磺胺喹啉(sulfaquinoxaline)Y=5.703×103X-3.025×1030.999 50.20.53.2
60磺胺噻唑(sulfathiazole)Y=7.445×103X-3.899×1030.999 90.20.525.4
61磺胺二甲异嘧啶(sulfisomidine)Y=9.322×103X-4.960×1030.999 30.20.537.7
62磺胺二甲异唑(sulphisoxazole)Y=9.831×103X-1.426×1040.999 90.20.522.1
63四环素(tetracycline)Y=6.682×101X-1.003×1020.999 00.41232.0
64替米考星(tilmicosin)Y=1.387×103X+1.013×1030.983 30.20.5-44.1
65甲砜霉素(thiamphenicol)Y=3.404×103X+6.654×1010.999 20.20.549.6
66替硝唑(tinidazole)Y=2.412×103X-1.238×1030.999 60.31-0.2
67甲氧苄啶(trimethoprim)Y=5.827×104X-1.980×1040.999 50.20.5-14.8
68五氯酚(pentachlorophenol)Y=5.808×103X+1.282×1040.999 50.20.510.2
), ArticleFig(id=1206300935672885973, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1206272758095344024, language=CN, label=表3, caption=

线性方程及相关系数(r)、检测限、定量限、基质效应

, figureFileSmall=null, figureFileBig=null, tableContent=
序号
(No.)
化合物
(compound)
线性方程
(linear equation)
rLOD/(ng · mL-1LOQ/(ng · mL-1基质效应
(matrix effect)/%
1金刚烷胺(amantadine)Y=1.081×105X+2.617×1040.999 90.20.5-8.7
2氯霉素(chloramphenicol)Y=1.093×103X+5.873×1020.998 20.20.5-14.6
3金霉素(chlortetracycline)Y=1.859×102X-4.225×1010.998 71516.8
4西诺沙星(cinoxacin)Y=1.080×105X-4.440×1040.998 90.20.5-42.2
5环丙沙星(ciprofloxacin)Y=1.670×104X+8.840×1030.999 30.31100.7
6克拉霉素(clarithromycin)Y=9.167×104X-3.971×1040.997 30.10.5-28.3
7丹氟沙星(canofloxacin)Y=6.002×104X-9.413×1030.999 50.3163.7
8双氟沙星(difloxacin)Y=3.505×104X-1.192×1040.999 60.41-3.9
9二甲硝咪唑(dimetridazole)Y=3.525×103X-2.211×1030.999 40.721.0
104,4’-二硝基均二苯脲
(4,4’-dinitrocarbanilide)
Y=1.171×104X-7.737×1020.999 60.10.5-13.2
11多西环素(doxycycline)Y=7.211×102X-1.790×1020.999 80.3117.7
12依诺沙星(enoxacin)Y=3.697×104X+9.790×1020.999 60.62108.5
13恩诺沙星(enrofloxacin)Y=6.618×104X-2.070×1040.999 60.31-6.8
14红霉素(erythromycin)Y=6.043×104X-3.631×1040.997 50.31-37.2
15氟虫腈(fipronil)Y=6.167×103X+3.109×1030.997 70.20.588.9
16氟甲腈(fipronil-desulfinyl)Y=2.348×104X-1.870×1030.999 70.20.59.0
17氟虫腈亚砜(fipronil-sulfide)Y=1.349×104X-3.591×1030.999 20.10.527.8
18氟虫腈砜(fipronil-sulfone)Y=1.383×104X-1.539×1030.999 70.20.5-4.6
19氟罗沙星(fleroxacin)Y=6.440×104X-5.630×1030.999 80.20.5-5.0
20氟苯尼考(florfenicol)Y=3.435×103X-1.217×1030.996 0310-7.3
21氟苯尼考胺(florfenicol amine)Y=5.787×103X+3.610×1030.996 10.20.55.2
22氟甲喹(flumequine)Y=1.649×105X-2.777×1040.998 30.41-17.4
23羟甲基甲硝咪唑(hydroxydimetridazole)Y=5.271×103X-2.453×1030.999 40.31-8.2
24羟基异丙硝唑(hydroxyipronidazole)Y=8.985×103X-4.000×1030.999 60.20.52.2
25羟基甲硝唑(hydroxymetronidazole)Y=8.474×102X+8.928×1010.997 40.20.5-49.9
26异丙硝唑(ipronidazole)Y=6.934×103X-2.813×1030.993 20.20.5-16.2
27林可霉素(lincomycin)Y=5.653×104X-4.586×1030.999 40.20.5-30.2
28洛美沙星(lomefloxacin)Y=3.706×105X-1.894×1030.999 90.41-1.5
29马波沙星(marbofloxacin)Y=8.297×104X-1.235×1040.999 40.314.6
30甲硝唑(metronidazole)Y=1.941×104X-1.081×1040.998 80.10.2-3.1
31诺氟沙星(norfloxacin)Y=1.409×104X+4.868×1030.999 50.31145.8
32氧氟沙星(ofloxacin)Y=8.826×104X-1.515×1040.999 30.3110.7
33奥比沙星(orbifloxacin)Y=6.713×104X-5.368×1030.999 30.20.5-14.7
34喹酸(oxolinic acid)Y=4.247×105X+9.243×1030.999 30.31-16.1
35土霉素(oxytetracycline)Y=3.259×102X-2.754×1020.999 70.7273.7
36培氟沙星(pefloxacin)Y=3.294×104X-5.310×1030.999 60.31-1.3
37金刚乙胺(rimantadine)Y=9.256×104X-5.884×1030.999 90.20.50.0
38罗红霉素(roxithromycin)Y=2.727×104X-1.180×1040.998 50.20.5-17.2
39沙拉沙星(sarafloxacin)Y=1.781×104X-3.932×1030.999 00.319.9
40司帕沙星(sparfloxacin)Y=6.255×104X-2.441×1040.999 70.31-10.7
41苯甲酰磺胺(sulfabenzamide)Y=9.860×103X-3.723×1030.999 90.20.5-2.5
42磺胺醋酰(sulfacetamide)Y=9.676×103X-2.522×1030.999 90.620.1
43磺胺氯哒嗪(sulfachloropyridazine)Y=4.746×103X-2.021×1030.999 80.20.511.4
44磺胺嘧啶(sulfadiazine)Y=9.565×103X-4.661×1030.999 90.20.511.2
45磺胺二甲氧嘧啶(sulfadimethoxine)Y=2.441×104X-1.383×1040.999 80.20.57.8
46磺胺二甲基嘧啶(sulfadimidine)Y=4.415×104X-1.646×1040.999 00.20.5-16.7
47磺胺邻二甲氧嘧啶(sulfadoxine)Y=1.315×104X-6.322×1030.999 70.20.5-0.7
48磺胺脒(sulfaguanidine)Y=8.070×103X-2.678×1030.999 80.20.51.5
49磺胺甲基嘧啶(sulfamerazine)Y=9.572×103X-3.500×1030.999 80.20.51.5
50磺胺对甲氧嘧啶(sulfameter)Y=1.969×104X-8.110×1030.999 70.20.525.8
51磺胺甲噻二唑(sulfamethizole)Y=6.058×103X-2.443×1030.999 60.20.51.5
52磺胺甲基异唑(sulfamethoxazole)Y=8.508×103X-4.536×1031.000 00.20.510.4
53磺胺甲氧哒嗪(sulfamethoxypyridazine)Y=1.055×103X-2.883×1020.999 10.72-15.1
54磺胺间甲氧嘧啶(sulfamonomethoxine)Y=4.919×103X-2.387×1030.999 90.20.53.9
55磺胺唑(sulfamoxole)Y=6.533×103X-2.688×1031.000 00.20.55.9
56磺胺硝苯(sulfanitran)Y=2.423×101X-5.3580.995 8210-25.8
57磺胺吡啶(sulfapyridine)Y=1.101×104X-9.653×1030.999 70.20.5-9.5
58磺胺苯吡唑(sulfaphenazole)Y=1.091×104X-3.947×1030.999 40.20.545.7
59磺胺喹啉(sulfaquinoxaline)Y=5.703×103X-3.025×1030.999 50.20.53.2
60磺胺噻唑(sulfathiazole)Y=7.445×103X-3.899×1030.999 90.20.525.4
61磺胺二甲异嘧啶(sulfisomidine)Y=9.322×103X-4.960×1030.999 30.20.537.7
62磺胺二甲异唑(sulphisoxazole)Y=9.831×103X-1.426×1040.999 90.20.522.1
63四环素(tetracycline)Y=6.682×101X-1.003×1020.999 00.41232.0
64替米考星(tilmicosin)Y=1.387×103X+1.013×1030.983 30.20.5-44.1
65甲砜霉素(thiamphenicol)Y=3.404×103X+6.654×1010.999 20.20.549.6
66替硝唑(tinidazole)Y=2.412×103X-1.238×1030.999 60.31-0.2
67甲氧苄啶(trimethoprim)Y=5.827×104X-1.980×1040.999 50.20.5-14.8
68五氯酚(pentachlorophenol)Y=5.808×103X+1.282×1040.999 50.20.510.2
), ArticleFig(id=1206300935786132186, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1206272758095344024, language=EN, label=Tab. 4, caption=

The results of recovery experiments

, figureFileSmall=null, figureFileBig=null, tableContent=
序号
(No.)
化合物
(compound)
低(low)中(middle)高(high)
回收率
(recovery)/%
RSD/%回收率
(recovery)/%
RSD/%回收率
(recovery)/%
RSD/%
1金刚烷胺(amantadine)110.01.6103.52.2106.01.6
2氯霉素(chloramphenicol)101.70.89101.91.1109.00.86
3金霉素(chlortetracycline)61.97.382.64.492.26.1
4西诺沙星(cinoxacin)101.42.994.54.8101.53.4
5环丙沙星(ciprofloxacin)92.91.093.12.799.91.0
6克拉霉素(clarithromycin)115.07.475.16.779.67.8
7丹氟沙星(canofloxacin)103.31.894.02.9103.71.3
8双氟沙星(difloxacin)95.93.890.54.698.71.9
9二甲硝咪唑(dimetridazole)*116.57.2111.75.9108.11.8
104,4’-二硝基均二苯脲(4,4’-dinitrocarbanilide)88.04.4104.71.599.71.8
11多西环素(doxycycline)110.12.797.22.4108.65.7
12依诺沙星(enoxacin)*90.63.683.35.085.45.3
13恩诺沙星(enrofloxacin)110.76.0103.33.8114.32.1
14红霉素(erythromycin)105.01.383.24.191.36.4
15氟虫腈(fipronil)108.06.6102.12.8101.01.1
16氟甲腈(fipronil-desulfinyl)108.43.296.41.599.41.5
17氟虫腈亚砜(fipronil-sulfide)112.92.6110.81.693.16.2
18氟虫腈砜(fipronil-sulfone)112.70.73112.63.985.43.1
19氟罗沙星(fleroxacin)106.08.2103.12.5104.72.0
20氟苯尼考(florfenicol)**106.22.3102.52.0109.51.8
21氟苯尼考胺(florfenicol amine)105.05.4101.52.197.02.8
22氟甲喹(flumequine)104.76.492.52.0102.92.0
23羟甲基甲硝咪唑(hydroxydimetridazole)111.31.4105.12.0108.11.8
24羟基异丙硝唑(hydroxyipronidazole)109.81.5105.40.95104.42.2
25羟基甲硝唑(hydroxymetronidazole)121.58.3115.87.6104.34.9
26异丙硝唑(ipronidazole)109.32.5104.60.56107.32.4
27林可霉素(lincomycin)101.54.286.00.98103.31.1
28洛美沙星(lomefloxacin)102.02.192.71.0100.11.0
29马波沙星(marbofloxacin)99.85.592.40.82107.21.0
30甲硝唑(metronidazole)85.55.778.44.965.96.2
31诺氟沙星(norfloxacin)102.25.396.45.9107.60.79
32氧氟沙星(ofloxacin)102.41.891.60.8198.40.98
33奥比沙星(orbifloxacin)99.44.4100.21.2100.01.8
34喹酸(oxolinic acid)97.72.2100.01.097.30.57
35土霉素(oxytetracycline)*92.62.784.90.9490.60.68
36培氟沙星(pefloxacin)94.15.990.85.198.24.1
37金刚乙胺(rimantadine)108.42.8101.11.3100.42.1
38罗红霉素(roxithromycin)97.61.1100.00.63100.11.2
39沙拉沙星(sarafloxacin)98.61.696.71.0104.61.2
40司帕沙星(sparfloxacin)106.02.797.91.6101.51.3
41苯甲酰磺胺(sulfabenzamide)111.41.4102.10.92101.11.0
42磺胺醋酰(sulfacetamide)*119.43.0118.00.80116.70.99
43磺胺氯哒嗪(sulfachloropyridazine)104.10.7598.00.97103.30.48
44磺胺嘧啶(sulfadiazine)96.22.097.60.8599.61.1
45磺胺二甲氧嘧啶(sulfadimethoxine)104.84.799.21.6101.41.0
46磺胺二甲基嘧啶(sulfadimidine)92.12.485.80.9790.51.7
47磺胺邻二甲氧嘧啶(sulfadoxine)99.75.698.33.8101.32.2
48磺胺脒(sulfaguanidine)104.41.098.40.9195.21.0
49磺胺甲基嘧啶(sulfamerazine)100.91.3100.02.8100.01.9
50磺胺对甲氧嘧啶(sulfameter)104.61.7103.02.0102.08.4
51磺胺甲噻二唑(sulfamethizole)99.71.895.41.5100.60.92
52磺胺甲基异唑(sulfamethoxazole)103.13.195.61.099.40.57
53磺胺甲氧哒嗪*(sulfamethoxypyridazine)111.95.885.81.689.42.5
54磺胺间甲氧嘧啶(sulfamonomethoxine)104.04.898.41.4100.91.2
55磺胺唑(sulfamoxole)103.93.392.81.298.70.90
56磺胺硝苯(sulfanitran)**97.76.695.96.097.75.3
57磺胺吡啶(sulfapyridine)105.85.198.42.4102.32.4
58磺胺苯吡唑(sulfaphenazole)113.54.1105.55.8108.41.8
59磺胺喹啉(sulfaquinoxaline)98.24.794.74.997.52.7
60磺胺噻唑(sulfathiazole)99.54.993.71.6100.51.4
61磺胺二甲异嘧啶(sulfisomidine)74.26.993.61.1104.71.3
62磺胺二甲异唑(sulphisoxazole)112.61.6116.72.2118.11.6
63四环素(tetracycline)101.70.8990.01.197.10.86
64替米考星(tilmicosin)102.77.3105.44.4102.46.1
65甲砜霉素(thiamphenicol)99.52.9100.64.8107.83.4
66替硝唑(tinidazole)102.91.0102.92.798.71.0
67甲氧苄啶(trimethoprim)112.77.4100.46.7103.57.8
68五氯酚(pentachlorophenol)104.31.899.42.9100.31.3
), ArticleFig(id=1206300935924544224, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1206272758095344024, language=CN, label=表4, caption=

回收率试验结果(n=6)

, figureFileSmall=null, figureFileBig=null, tableContent=
序号
(No.)
化合物
(compound)
低(low)中(middle)高(high)
回收率
(recovery)/%
RSD/%回收率
(recovery)/%
RSD/%回收率
(recovery)/%
RSD/%
1金刚烷胺(amantadine)110.01.6103.52.2106.01.6
2氯霉素(chloramphenicol)101.70.89101.91.1109.00.86
3金霉素(chlortetracycline)61.97.382.64.492.26.1
4西诺沙星(cinoxacin)101.42.994.54.8101.53.4
5环丙沙星(ciprofloxacin)92.91.093.12.799.91.0
6克拉霉素(clarithromycin)115.07.475.16.779.67.8
7丹氟沙星(canofloxacin)103.31.894.02.9103.71.3
8双氟沙星(difloxacin)95.93.890.54.698.71.9
9二甲硝咪唑(dimetridazole)*116.57.2111.75.9108.11.8
104,4’-二硝基均二苯脲(4,4’-dinitrocarbanilide)88.04.4104.71.599.71.8
11多西环素(doxycycline)110.12.797.22.4108.65.7
12依诺沙星(enoxacin)*90.63.683.35.085.45.3
13恩诺沙星(enrofloxacin)110.76.0103.33.8114.32.1
14红霉素(erythromycin)105.01.383.24.191.36.4
15氟虫腈(fipronil)108.06.6102.12.8101.01.1
16氟甲腈(fipronil-desulfinyl)108.43.296.41.599.41.5
17氟虫腈亚砜(fipronil-sulfide)112.92.6110.81.693.16.2
18氟虫腈砜(fipronil-sulfone)112.70.73112.63.985.43.1
19氟罗沙星(fleroxacin)106.08.2103.12.5104.72.0
20氟苯尼考(florfenicol)**106.22.3102.52.0109.51.8
21氟苯尼考胺(florfenicol amine)105.05.4101.52.197.02.8
22氟甲喹(flumequine)104.76.492.52.0102.92.0
23羟甲基甲硝咪唑(hydroxydimetridazole)111.31.4105.12.0108.11.8
24羟基异丙硝唑(hydroxyipronidazole)109.81.5105.40.95104.42.2
25羟基甲硝唑(hydroxymetronidazole)121.58.3115.87.6104.34.9
26异丙硝唑(ipronidazole)109.32.5104.60.56107.32.4
27林可霉素(lincomycin)101.54.286.00.98103.31.1
28洛美沙星(lomefloxacin)102.02.192.71.0100.11.0
29马波沙星(marbofloxacin)99.85.592.40.82107.21.0
30甲硝唑(metronidazole)85.55.778.44.965.96.2
31诺氟沙星(norfloxacin)102.25.396.45.9107.60.79
32氧氟沙星(ofloxacin)102.41.891.60.8198.40.98
33奥比沙星(orbifloxacin)99.44.4100.21.2100.01.8
34喹酸(oxolinic acid)97.72.2100.01.097.30.57
35土霉素(oxytetracycline)*92.62.784.90.9490.60.68
36培氟沙星(pefloxacin)94.15.990.85.198.24.1
37金刚乙胺(rimantadine)108.42.8101.11.3100.42.1
38罗红霉素(roxithromycin)97.61.1100.00.63100.11.2
39沙拉沙星(sarafloxacin)98.61.696.71.0104.61.2
40司帕沙星(sparfloxacin)106.02.797.91.6101.51.3
41苯甲酰磺胺(sulfabenzamide)111.41.4102.10.92101.11.0
42磺胺醋酰(sulfacetamide)*119.43.0118.00.80116.70.99
43磺胺氯哒嗪(sulfachloropyridazine)104.10.7598.00.97103.30.48
44磺胺嘧啶(sulfadiazine)96.22.097.60.8599.61.1
45磺胺二甲氧嘧啶(sulfadimethoxine)104.84.799.21.6101.41.0
46磺胺二甲基嘧啶(sulfadimidine)92.12.485.80.9790.51.7
47磺胺邻二甲氧嘧啶(sulfadoxine)99.75.698.33.8101.32.2
48磺胺脒(sulfaguanidine)104.41.098.40.9195.21.0
49磺胺甲基嘧啶(sulfamerazine)100.91.3100.02.8100.01.9
50磺胺对甲氧嘧啶(sulfameter)104.61.7103.02.0102.08.4
51磺胺甲噻二唑(sulfamethizole)99.71.895.41.5100.60.92
52磺胺甲基异唑(sulfamethoxazole)103.13.195.61.099.40.57
53磺胺甲氧哒嗪*(sulfamethoxypyridazine)111.95.885.81.689.42.5
54磺胺间甲氧嘧啶(sulfamonomethoxine)104.04.898.41.4100.91.2
55磺胺唑(sulfamoxole)103.93.392.81.298.70.90
56磺胺硝苯(sulfanitran)**97.76.695.96.097.75.3
57磺胺吡啶(sulfapyridine)105.85.198.42.4102.32.4
58磺胺苯吡唑(sulfaphenazole)113.54.1105.55.8108.41.8
59磺胺喹啉(sulfaquinoxaline)98.24.794.74.997.52.7
60磺胺噻唑(sulfathiazole)99.54.993.71.6100.51.4
61磺胺二甲异嘧啶(sulfisomidine)74.26.993.61.1104.71.3
62磺胺二甲异唑(sulphisoxazole)112.61.6116.72.2118.11.6
63四环素(tetracycline)101.70.8990.01.197.10.86
64替米考星(tilmicosin)102.77.3105.44.4102.46.1
65甲砜霉素(thiamphenicol)99.52.9100.64.8107.83.4
66替硝唑(tinidazole)102.91.0102.92.798.71.0
67甲氧苄啶(trimethoprim)112.77.4100.46.7103.57.8
68五氯酚(pentachlorophenol)104.31.899.42.9100.31.3
), ArticleFig(id=1206300936021013222, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1206272758095344024, language=EN, label=Tab. 5, caption=

The detection results of positive sample

, figureFileSmall=null, figureFileBig=null, tableContent=
样品编号
(sample No.)
兽药残留(veterinary drug residues)/(μg · kg-1
金刚烷胺
(amantadine)
多西环素
(doxycycline)
恩诺沙星
(enrofloxacin)
氟苯尼考
(florfenicol)
S225ND57ND*
S9NDNDND67
S28NDND67ND
S33NDNDND37
S37ND48NDND
), ArticleFig(id=1206300936142648045, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1206272758095344024, language=CN, label=表5, caption=

阳性样品检测结果

, figureFileSmall=null, figureFileBig=null, tableContent=
样品编号
(sample No.)
兽药残留(veterinary drug residues)/(μg · kg-1
金刚烷胺
(amantadine)
多西环素
(doxycycline)
恩诺沙星
(enrofloxacin)
氟苯尼考
(florfenicol)
S225ND57ND*
S9NDNDND67
S28NDND67ND
S33NDNDND37
S37ND48NDND
), ArticleFig(id=1206300936239117044, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1206272758095344024, language=EN, label=Tab. 6, caption=

Veterinary drug residues of positive samples after processing

, figureFileSmall=null, figureFileBig=null, tableContent=
样品编号
(sample number)
炮制后兽药残留(veterinary drug residues after processing)/(μg · kg-1
金刚烷胺
(amantadine)
多西环素
(doxycycline)
恩诺沙星
(enrofloxacin)
氟苯尼考
(florfenicol)
S217ND30ND
S9NDNDND33
S28NDND28ND
S33NDNDND18
S37ND21NDND
), ArticleFig(id=1206300936323003128, tenantId=1146029695717560320, journalId=1205117023404326918, articleId=1206272758095344024, language=CN, label=表6, caption=

阳性样品炮制后兽药残留

, figureFileSmall=null, figureFileBig=null, tableContent=
样品编号
(sample number)
炮制后兽药残留(veterinary drug residues after processing)/(μg · kg-1
金刚烷胺
(amantadine)
多西环素
(doxycycline)
恩诺沙星
(enrofloxacin)
氟苯尼考
(florfenicol)
S217ND30ND
S9NDNDND33
S28NDND28ND
S33NDNDND18
S37ND21NDND
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固相萃取-UPLC-MS/MS同时测定鸡内金中68种兽药残留*
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刘萌 , 张亮 , 陈芳芳 , 李志梅 ** , 张崇生
药物分析杂志 | 安全监测 2025,45(5): 889-900
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药物分析杂志 | 安全监测 2025, 45(5): 889-900
固相萃取-UPLC-MS/MS同时测定鸡内金中68种兽药残留*
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刘萌 , 张亮, 陈芳芳, 李志梅** , 张崇生
作者信息
  • 温州市食品药品检验科学研究院,温州 325000
  • Tel:13587627800;E-mail:

通讯作者:

** Tel:13587409531;E-mail:
UPLC-QQQ MS/MS with solid phase extraction for simultaneous determination of 68 veterinary drug residues in Galli Gigerii Endothelium Corneum
Meng LIU , Liang ZHANG, Fang-fang CHEN, Zhi-mei LI** , Chong-sheng ZHANG
Affiliations
  • Wenzhou Research Institute for Food and Drug Control, Wenzhou 325000, China
doi: 10.16155/j.0254-1793.2024-1214
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目的:建立固相萃取-超高效液相色谱串联三重四极杆质谱法(UPLC-QQQ MS/MS法)测定中药鸡内金中68种兽药残留。方法:样品匀质后,经乙腈和含0.5%甲酸的乙腈进行2次提取,并经Oasis PRiME HLB固相萃取柱净化。采用Agilent ZORBAX Eclipse Plus C18(3.0 mm×150 mm,1.8 μm)色谱柱分离,以乙腈和5 mmol · L-1乙酸铵水溶液(含0.1%甲酸)体系为流动相进行梯度洗脱;ESI电离源,正、负离子模式,多反应监测(MRM),空白基质匹配标准曲线法定量。结果:68种兽药在一定质量浓度范围内线性关系良好,r≥0.995 8;方法检测限(LOD)为0.1~3 μg · kg-1,定量限(LOQ)为0.2~10 μg · kg-1;3个浓度水平下(n=6)加样回收率在61.9%~121.5%,RSD为0.50%~8.4%。在50批鸡内金样品中共有5批检出兽药残留,检出的兽药残留包括金刚烷胺、多西环素、恩诺沙星、氟苯尼考。结论:本方法简便、快捷、准确、可靠,适用于鸡内金中多种兽药残留的测定。

固相萃取  /  超高效液相色谱串联质谱  /  兽药残留  /  鸡内金

Objective: To establish a method for the determination of veterinary drug residues in Galli Gigerii Endothelium Corneum by ultra high performance liquid chromatography-tandem triple quadrupole mass spectrometry (UPLC-QQQ MS/MS) with solid-phase extraction. Methods: The samples were evenly dispersed,extracted with acetonitrile and acetonitrile containing 0.5% formic acid, and cleaned up with Oasis PRiME HLB solid phase extraction columns. The extracts were separated on Agilent ZORBAX Eclipse Plus C18 (3.0 mm×150 mm, 1.8 μm) using 5 mmol · L-1 ammonium acetate and acetonitrile (containing 0.1% formic acid) as mobile phase by gradient elution. The detection of veterinary drug residues was detected by tandem mass spectrometry with positive electrospray ion source under multiple reaction monitoring (MRM) mode. The matrix-matched external standard method was used for the quantitation. Results: The method exhibited good linearities within a certain concentration range r≥0.995 8. The limits of detection (LODs) were in the range of 0.1-3 μg · kg-1. The limits of quantitation (LOQs) were in the range of 0.2-10 μg · kg-1. The good recovery values (61.9%-121.5%) were achieved for all the 68 veterinary drugs with RSDs ranging from 0.50% to 8.4% for spiking 3 different levels. Out of 50 batches of samples, 5 batches of Galli Gigerii Endothelium Corneum were found to contain veterinary drug residues,including amantadine, doxycycline, enrofloxacin, and florfenicol. Conclusion: This method proves suitable for the rapid determination of multiple veterinary drug residues in Galli Gigerii Endothelium Corneum, with a simple,quick, accurate and procedure.

solid phase extraction  /  ultra high performance liquid chromatography-tandem triple quadrupole mass spectrometry (UPLC-QQQ MS/MS)  /  veterinary drug residues  /  Galli Gigerii Endothelium Corneum
刘萌, 张亮, 陈芳芳, 李志梅, 张崇生. 固相萃取-UPLC-MS/MS同时测定鸡内金中68种兽药残留*. 药物分析杂志, 2025 , 45 (5) : 889 -900 . DOI: 10.16155/j.0254-1793.2024-1214
Meng LIU, Liang ZHANG, Fang-fang CHEN, Zhi-mei LI, Chong-sheng ZHANG. UPLC-QQQ MS/MS with solid phase extraction for simultaneous determination of 68 veterinary drug residues in Galli Gigerii Endothelium Corneum[J]. Chinese Journal of Pharmaceutical Analysis, 2025 , 45 (5) : 889 -900 . DOI: 10.16155/j.0254-1793.2024-1214
鸡内金又名鸡食皮、鸡合子、化石胆,《神农本草经》记载其有健胃消食、涩精止遗、通淋化石的功效,常用于食积不消、呕吐泻痢、小儿疳积、遗尿、遗精、石淋涩痛、胆胀胁痛[1],是我国传统消导药之一,可药食兼用,是应用较为广泛的一种中药饮片。据统计,269 882张内科处方中,鸡内金使用频率达9.68%,排在内科用药频率的第35位[2]。2020年版《中华人民共和国药典》 (简称《中国药典》)和陕西、北京、江西、广西、湖南、浙江、上海七地的《中药饮片炮制规范》均有收载。2020年版《中国药典》规定,鸡内金为雉科动物家鸡Gallus gallus domesticusBrisson的干燥沙囊内壁[3]。杀鸡后,取出鸡肫,立即剥下内壁,洗净,干燥,其炮制方法包括清炒、烫法、砂炒法、醋制法、盐炙。2020年版《中国药典》收载的炮制品包括炒鸡内金和醋鸡内金,2015年版《浙江省中药炮制规范》收载的炮制品有炒鸡内金。鸡内金的原料来自饲养家鸡,其养殖和产地初加工普遍缺乏统一的标准化操作规程,为提高家鸡的产量,养殖环节经常使用各类兽药。根据《食品安全国家标准》GB31650-2019,其中39种兽药只是在产蛋期禁用,且标准只对其在动物性食品中的最高残留限量进行了规定,存在部分兽药滥用、误用和不遵守休药期等现象。根据2014—2022年国家市场监督管理总局对鸡肉抽检结果统计[4],发现兽药残留检出率为1.5%,主要检出兽药包括五氯酚、尼卡巴嗪、呋喃唑酮代谢物、土霉素、恩诺沙星、金刚烷胺等,其中,五氯酚和恩诺沙星是近3年来检出频率最高的兽药。虽然《食品安全国家标准》GB31650-2019规定了食品中兽药最大残留限量,但是2020年版《中国药典》未对动物类中药中的兽药残留进行规定,因此,有必要对鸡内金等动物类中药饮片中的兽药残留进行监测和控制。
目前,液相色谱-质谱分析方法已成为同时检测多种兽药残留的重要手段[5]。随着质谱检测技术的发展,质谱的类型逐渐由单级转向多级,相对于单级质谱,多级质谱具有灵敏度强,选择性高等优势。例如,四极杆-飞行时间质谱法[6-8]、三重四极杆串联质谱法[9-10]。为了去除杂质干扰、提高检测灵敏度、降低基质效应,QuEChERS法被广泛应用于兽药残留检测的样品前处理[11-13]
本研究采用不同酸度的乙腈进行2次提取,提取液经固相萃取柱净化,采用超高效液相色谱-串联三重四极杆质谱(UPLC-QQQ MS/MS)技术,建立了鸡内金中多种兽药残留的检测方法,用于实际样品的定量分析,并评价炮制对鸡内金中兽药残留的影响。
Agilent 1290/6470 UPLC-MS/MS液相色谱-串联质谱仪,配ESI源(Agilent 公司),MS3BS025漩涡混合器(IKA 公司),XS205DU十万分之一电子天平(Metler Toledo 公司),CF16RXⅡ离心机(HITACHI公司);Oasis PRiME HLB固相萃取柱(Waters 公司)。
甲醇、乙腈、乙酸均为色谱纯(Merck 公司);水为超纯水;68种兽药对照品:金刚烷胺(纯度99.8%)、氯霉素(纯度99.3%)、金霉素(纯度93.4%)、西诺沙星(纯度99.9%)、环丙沙星(纯度99.4%)、克拉霉素(纯度97.8%)、丹氟沙星(纯度98.1%)、双氟沙星(纯度94.5%)、二甲硝咪唑(纯度98.9%)、4,4’-二硝基均二苯脲(纯度95.7%)、盐酸多西环素(纯度93.4%)、依诺沙星(纯度92.7%)、恩诺沙星(纯度99.8%)、红霉素(纯度98.4%)、氟虫腈(纯度98.3%)、氟甲腈(纯度93.3%)、氟虫腈亚砜(纯度99.8%)、氟虫腈砜(纯度99.4%)、氟罗沙星(纯度99.7%)、氟苯尼考(纯度99.1%)、氟苯尼考胺(纯度99.9%)、氟甲喹(纯度99.4%)、羟甲基甲硝咪唑(纯度99.4%)、羟基异丙硝唑(纯度98.9%)、羟基甲硝唑(纯度99.5%)、林可霉素(纯度95.8%)、洛美沙星(纯度96.0%)、马波沙星(纯度99.9%)、甲硝唑(纯度99.8%)、诺氟沙星(纯度98.1%)、氧氟沙星(纯度99.8%)、奥比沙星(纯度96.8%)、恶喹酸(纯度99.2%)、土霉素盐酸盐(纯度94.3%)、培氟沙星(纯度99.7%)、金刚乙胺盐酸盐(纯度99.6%)、罗红霉素(纯度96.8%)、司帕沙星(纯度99.7%)、苯甲酰磺胺(纯度98.9%)、磺胺醋酰(纯度99.3%)、磺胺氯哒嗪(纯度99.1%)、磺胺嘧啶(纯度99.7%)、磺胺二甲氧嘧啶(纯度98.0%)、磺胺二甲基嘧啶(纯度99.5%)、磺胺邻二甲氧嘧啶(纯度99.7%)、磺胺脒(纯度92.1%)、磺胺甲基嘧啶(纯度99.5%)、磺胺对甲氧嘧啶(纯度99.7%)、磺胺甲噻二唑(纯度98.0%)、磺胺甲基异唑(纯度98.3%)、磺胺甲氧哒嗪(纯度99.2%)、磺胺间甲氧嘧啶(纯度98.2%)、磺胺唑(纯度98.0%)、磺胺硝苯(纯度97.3%)、磺胺吡啶(纯度99.7%)、磺胺喹啉(纯度96.4%)、磺胺噻唑(纯度96.3%)、磺胺二甲异嘧啶(纯度95.0%)、磺胺二甲异唑(纯度97.3%)、四环素盐酸盐(纯度97.7%)、替米考星(纯度98.5%)、甲砜霉素(纯度99.8%)、替硝唑(纯度99.9%)、甲氧苄啶(纯度99.8%)、沙拉沙星(纯度91.0%)、五氯酚(纯度91.1%),均购于上海安谱实验科技股份有限公司。
50批鸡内金采购于温州地区药品零售企业及药品批发企业,由温州市食品药品检验科学研究院按2020年版《中国药典》或2015年版《浙江省中药炮制规范》检验,结果均符合规定,其质量标准及炮制情况见表1
采用Agilent ZORBAX Eclipse Plus C18(3.0 mm×150 mm,1.8 μm)色谱柱,以乙腈(含0.1%甲酸)为流动相A,5 mmol · L-1乙酸铵水溶液(含0.1%甲酸)为流动相B,梯度洗脱(0~0.5 min,2%A;0.5~1.8 min,2%A→15%A;1.8~3.5 min,15%A→20%A;3.5~6 min,20 %A→25%A;6~7 min,25%A→30%A;7~11 min,30%A→35%A;11~16 min,35%A→100%A;16~26 min,100%A),流速0.45 mL · mim-1,柱温45 ℃,进样量5 μL。
离子源:ESI电离源,正、负离子模式,离子源温度350 ℃,干燥气温度325 ℃,干燥气流速8 L · min-1;雾化器压力310 kPa,毛细管电压4 000 V,喷嘴电压500 V,碎裂电压166 V,鞘气温度350℃,鞘气流速12 L · min-1,监测模式为多反应监测(MRM)。68种兽药质谱采集参数见表2
分别取68种兽药对照品适量,加甲醇溶解并稀释成质量浓度为1.0 mg · mL-1的对照品储备液,-18 ℃储存3个月。临用前分别吸取各兽药对照品储备液适量混合,用甲醇稀释成质量浓度为1 μg · mL-1的混合对照品溶液。
取鸡内金粉末(过120目筛)约2 g,精密称定,置于离心管中,精密加入麦氏缓冲液(pH 5.0)5 mL,加入3 mm不锈钢珠2粒,涡旋混合 1 min 后,再精密加入乙腈10 mL,涡旋混合1 min,加入氯化钠1 g和硫酸钠4 g,8 000 r · min-1离心5 min。精密量取上清液2 mL,待用。在离心管中精密加入含1%甲酸的乙腈2 mL,涡旋混合1 min,8 000 r · min-1离心5 min,精密量取上清液2 mL,与第1次提取的上清液合并。过Oasis PRiME HLB固相萃取柱,重力自流,收集流出液,用80%乙腈3 mL冲洗萃取小柱,合并流出液。流出液于45 ℃氮吹近干,加60%乙腈1 mL复溶,涡旋混合1 min,过 0. 22 µm PTFE滤膜,作为供试品溶液。取“2.3”项下不同体积的混合对照品溶液,并用空白样品同法制成的空白基质溶液,稀释制成基质匹配标准溶液,用于UPLC-MS/MS分析。
精密取“2.3”项下不同体积混合对照品溶液适量,用空白基质溶液配制成质量浓度分别为0、1、5、10、20、50、200 ng · mL-1的系列对照品溶液,进样测定。采用外标定量法,以各化合物浓度为横坐标,各化合物定量离子响应值为纵坐标,进行线性回归,得标准曲线;以信噪比均>3时的浓度为检测限,信噪比均>10时的浓度为定量限。结果见表3
基质效应是由于基质共提物与目标化合物在离子源中竞争电离,影响目标化合物响应强度的现象,影响定量分析结果的准确性和可靠性。取“2.3”项下系列浓度混合对照品溶液和“2.4”项下基质匹配标准溶液,按“2.1”“2.2”项下条件注入仪器,以各化合物的质量浓度X为横坐标,各成分峰面积Y为纵坐标,绘制标准曲线,并计算基质效应。基质效应(ME)=(基质匹配混合标准溶液标准曲线的斜率/无基质匹配混合标准溶液曲线斜率-1)×100%,结果见表3。ME<0,表示存在抑制效应;ME>0,表示存在增强效应;当ME在-20%~20%时,表示基质效应不明显[14]。本文中共有21个化合物存在明显基质效应,因此,采用空白基质匹配标准曲线用于定量计算,以确保测定结果准确。
取空白样品2.0 g,共18份,按低、中、高3个加样水平,分别加入质量浓度为1 μg · mL-1的混合对照品溶液2、100、200 μL,即添加水平分别为1、50、100 μg · kg-1,进行回收率试验,计算各添加水平的收率和RSD,结果见表4
表1中的鸡内金样品,按“2.4”项下方法配制供试品溶液并在本文色谱、质谱条件下进行测定,其中5批样品检出兽药残留,检出率为8.3%(表5)。检出的兽药残留主要包括喹诺酮类抗生素、抗病毒药物等。检出兽药残留种类及检出率与我国多地鸡肉中兽药残留监测结果[15-16]相符。
肌肉等蛋白质含量较高的样品中兽药残留的提取溶剂主要为乙腈,并通过加入低浓度的EDTA避免兽药和金属离子的络合[17]。但由于鸡内金细粉含水量低,先用含EDTA的麦氏缓冲液(pH 5.0)对其进行浸泡,有利于提取溶剂渗入及降低杂质干扰,利于后续溶剂提取。对于喹诺酮类等两性化合物,加入低浓度的甲酸,可提高兽药在提取溶剂中溶解度[18]。本文对比乙腈中添加不同浓度甲酸(0.1%、0.2%、0.5%、1%)对68种兽药回收率的影响,发现含0.2%甲酸的乙腈对喹诺酮类、四环素类等目标化合物具有最佳提取效果,回收率在80%~120%。但大多数磺胺类化合物回收率<60%,可能是由于磺胺类为弱碱性化合物,在过高的酸性环境中提取会产生相当程度的损失。本文采用2次提取的方式,即分别采用乙腈和含0.2%甲酸的乙腈进行提取,合并提取液,用于后续净化。经过2次提取,大多数目标化合物的回收率在80%~120%。
动物源性样品中兽药残留测定时,常选择C18、PSA[19]、Oasin PRiME HLB[20]、Bond Elut HLB SPE作为净化萃取柱,基于待测物质不被填料吸附,而磷脂、蛋白质、脂肪等干扰物被吸附于固相萃取填料的特性,实现样液分离与净化。本文选择以上4种净化方式,比较其对净化效果的影响,结果表明,Oasin PRiME HLB对大多数目标化合物回收率在80%~120%,净化效果最佳。其原因可能是鸡内金几乎不含脂肪,主要成分为蛋白质和磷脂,Oasin PRiME HLB对长链结构物质(如磷脂、游离脂肪酸、甘油三酯等)具有较强的吸附作用[21]
50批样品测定结果显示,炒鸡内金中均未检出兽药残留。根据2020年版《中国药典》,炒鸡内金由鸡内金清炒或烫法炒至鼓起[3]。文献报道的炒鸡内金炮制工艺有:炒制时间120 s,炒制温度215 ℃ ;金沙烫锅底温度200~201 ℃,炮制时间60 s;200 ℃烤制5 min[22]。由于炒鸡内金的炮制温度达200 ℃以上,因此,鸡内金的炒制过程可能会引起兽药分解。本文制备兽药残留量200 μg · kg-1鸡内金模拟样品,考察其在200 ℃加热不同时间后兽药残留量的变化,结果(图1)大部分兽药残留量可以在200 ℃加热5 min时明显下降,但不同种类兽药残留量降解速度差异较大,其中,四环素类抗生素降解较为显著。
将“2.6”项下阳性样品按照文献[22]报道的炮制工艺,于200 ℃烤制5 min,比较炮制前后兽药残留量变化,结果见表6。发现兽药残留虽明显减少,但仍高于定量限。
本文建立了鸡内金中68种兽药残留测定方法,通过不同酸碱性溶剂进行2次提取,并经固相萃取柱净化和UPLC-MS/MS法分析。该方法操作简便、快速,净化效果好,灵敏度高,准确度好,可以用于动物类中药的兽药残留研究和监管。同时也发现,炒制可以降低鸡内金兽药残留量,为鸡内金的炮制工艺优化提供了依据。
  • *浙江省市场监督管理局雏鹰计划核心项目(CY2022227)
  • 温州市重大科技创新攻关项目(ZN2021002)
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doi: 10.16155/j.0254-1793.2024-1214
  • 接收时间:2024-10-18
  • 首发时间:2025-12-12
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  • 收稿日期:2024-10-18
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*浙江省市场监督管理局雏鹰计划核心项目(CY2022227)
温州市重大科技创新攻关项目(ZN2021002)
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    温州市食品药品检验科学研究院,温州 325000

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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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