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Article(id=1193674740968682493, tenantId=1146029695717560320, journalId=1190317699101192196, issueId=1193674740352119804, articleNumber=1001-2494(2025)06-0638-08, orderNo=null, doi=10.11669/cpj.2025.06.010, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1726070400000, receivedDateStr=2024-09-12, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1762523835650, onlineDateStr=2025-11-07, pubDate=1742572800000, pubDateStr=2025-03-22, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1762523835650, onlineIssueDateStr=2025-11-07, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1762523835650, creator=13701087609, updateTime=1762523835650, updator=13701087609, issue=Issue{id=1193674740352119804, tenantId=1146029695717560320, journalId=1190317699101192196, year='2025', volume='60', issue='6', pageStart='553', pageEnd='662', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1762523835503, creator=13701087609, updateTime=1762524041683, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1193675605205025683, tenantId=1146029695717560320, journalId=1190317699101192196, issueId=1193674740352119804, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1193675605205025684, tenantId=1146029695717560320, journalId=1190317699101192196, issueId=1193674740352119804, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=638, endPage=645, ext={EN=ArticleExt(id=1193674742117921791, articleId=1193674740968682493, tenantId=1146029695717560320, journalId=1190317699101192196, language=EN, title=Screening Analysis and Limit Standard Study of 99 Pesticides in Atractylodis Macrocephalae Rhizoma, columnId=null, journalTitle=Chinese Pharmaceutical Journal, columnName=null, runingTitle=null, highlight=null, articleAbstract=

OBJECTIVE To explore the development of maximum residue limit standards for pesticides in Atractylodis Macrocephalae Rhizoma that conform to the characteristics of traditional Chinese medicine use. METHODS The samples were processed by QuEChERS method, and a combination of GC-MS/MS and LC-MS/MS was used to screen and determine 99 pesticide indicators in Atractylodis Macrocephalae Rhizoma. At the same time, the sensitivity, recovery rate, reproducibility, and precision of the method were verified. A risk assessment model and transformation principle that conforms to the characteristics of traditional Chinese medicine were adopted to determine the indicators and limits of the pesticide limit standards for Atractylodis Macrocephalae Rhizoma. RESULTS The established method for determining 99 pesticides in Atractylodis Macrocephalae Rhizoma meets the methodological requirements. A total of 12 pesticides were detected in 53 batches of Atractylodis Macrocephalae Rhizoma samples, including: tebuconazole, benzofenapyr, cypermethrin and S-cypermethrin, pyraclostrobin, thiamethoxam, enoxymorpholine, diazinon, propiconazole, fipronil, and methoxam. According to the GB2763 conversion guidelines, the limit standard for diazinon in Atractylodis Macrocephalae Rhizoma was converted into a drug standard. CONCLUSION This study helps to understand the risk of pesticide residues in Atractylodis Macrocephalae Rhizoma and provides ideas for the formulation of pesticide residue limit standards for traditional Chinese medicine.

, correspAuthors=Ying WANG, Xiaoxiao LIU, authorNote=null, correspAuthorsNote=null, copyrightStatement=null, 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=Wanqing ZHANG, Yuanxi LIU, Hongyu JIN, Zhen LIU, Ying WANG, Shuangcheng MA, Xiaoxiao LIU), CN=ArticleExt(id=1193674742520573956, articleId=1193674740968682493, tenantId=1146029695717560320, journalId=1190317699101192196, language=CN, title=白术中99种农药筛查分析及限量标准研究, columnId=1190352405612040510, journalTitle=中国药学杂志, columnName=论著, runingTitle=null, highlight=null, articleAbstract=

目的 探索制定符合中药使用特点的白术中农药最大残留限量标准。方法 样品经QuEChERS法处理,采用气相色谱-串联质谱联用(GC-MS/MS)和液相色谱-串联质谱联用(LC-MS/MS)结合的方法对白术中99种农药指标进行筛查测定,同时对方法的灵敏度、回收率、重现性、精密度进行验证;采用符合中药特点的风险评估模式及转化原则,确定白术农药限量标准的指标及限度。结果 建立的白术中99种农药测定法符合方法学要求;53批白术样品中共检出农药12种,分别为:戊唑醇、苯醚甲环唑、氰戊菊酯和S-氰戊菊酯、吡唑醚菌酯、噻呋酰胺、烯酰吗啉、二嗪磷、双炔酰菌胺、精甲霜灵、丙环唑、氟虫腈、甲拌磷;按照GB2763转化指导原则将白术中二嗪磷限量标准转化为药品标准。结论 本研究有助于了解白术农药残留现状,可为其他中药品种农药残留限量标准的制定提供思路。

, correspAuthors=王莹, 刘潇潇, authorNote=null, correspAuthorsNote=
*王莹,女,博士,副研究员 研究方向:中药质量与安全 Tel:(010)53851413;
刘潇潇,女,博士,主任药师 研究方向:中药质量与安全 Tel:(020)32447998
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张万青,男,主管中药师 研究方向:中药农药残留检测与风险评估

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张万青,男,主管中药师 研究方向:中药农药残留检测与风险评估

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张万青,男,主管中药师 研究方向:中药农药残留检测与风险评估

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journalId=1190317699101192196, articleId=1193674740968682493, language=CN, orderNo=5, keyword=二嗪磷)], refs=[Reference(id=1193712702162956730, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193674740968682493, doi=null, pmid=null, pmcid=null, year=2020, volume=null, issue=null, pageStart=107, pageEnd=108, url=null, language=null, rfNumber=[1], rfOrder=0, authorNames=null, journalName=Ch.P(2020) Vol Ⅰ(中国药典2020年版.一部), refType=null, unstructuredReference=Ch.P(2020) Vol Ⅰ(中国药典2020年版.一部)[S]. 2020: 107-108., articleTitle=null, refAbstract=null), Reference(id=1193712702246842811, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193674740968682493, doi=null, pmid=null, pmcid=null, year=2022, volume=57, issue=10, pageStart=784, pageEnd=790, url=null, language=null, rfNumber=[2], rfOrder=1, authorNames=LUO Y Y, QIAN X W, SHA X X, journalName=Chin Pharm J(中国药学杂志), refType=null, unstructuredReference=LUO Y Y, QIAN X W, SHA X X, et al. 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China Pesticide Information Network, 2024 [2024-06-20]. http://jd100.chinapesticide.org.cn/zwb/dataCenter., articleTitle=Pesticide registration data, refAbstract=null), Reference(id=1193712702850822594, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193674740968682493, doi=null, pmid=null, pmcid=null, year=2023, volume=58, issue=15, pageStart=1416, pageEnd=1421, url=null, language=null, rfNumber=[9], rfOrder=8, authorNames=WANG Y, LIU Y X, ZHENG Z T, journalName=Chin Pharm J(中国药学杂志), refType=null, unstructuredReference=WANG Y, LIU Y X, ZHENG Z T, et al. A preliminary study on the principle of conversion of limit standards of traditional chinese medicine in “GB2763 national food safety standard-maximum residue limits for pesticides in food”[J]. 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National food safety standard: maximum residue limits for pesticides in food[S]. 2021., articleTitle=null, refAbstract=null), Reference(id=1193712702993428932, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193674740968682493, doi=null, pmid=null, pmcid=null, year=2020, volume=null, issue=null, pageStart=520, pageEnd=522, url=null, language=null, rfNumber=[11], rfOrder=10, authorNames=null, journalName=Ch.P(2020) Vol Ⅳ(中国药典 2020 年版. 四部), refType=null, unstructuredReference=Ch.P(2020) Vol Ⅳ(中国药典 2020 年版. 四部)[S]. 2020: 520-522., articleTitle=null, refAbstract=null), Reference(id=1193712703081509317, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193674740968682493, doi=null, pmid=null, pmcid=null, year=2023, volume=25, issue=6, pageStart=1179, pageEnd=1186, url=null, language=null, rfNumber=[12], rfOrder=11, authorNames=ZUO T T, LIU J, WANG Y, journalName=Mod Chin Med(中国现代中药), refType=null, unstructuredReference=ZUO T T, LIU J, WANG Y, et al. Research progress and prospect of risk assessment system for exogenous harmful substances and endogenous toxic components in Chinese medicinal materials[J]. Mod Chin Med(中国现代中药), 2023, 25(6):1179-1186., articleTitle=Research progress and prospect of risk assessment system for exogenous harmful substances and endogenous toxic components in Chinese medicinal materials, refAbstract=null), Reference(id=1193712703152812486, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193674740968682493, doi=null, pmid=null, pmcid=null, year=2024, volume=25, issue=3, pageStart=251, pageEnd=256, url=null, language=null, rfNumber=[13], rfOrder=12, authorNames=ZHANG W Q, LIU Y X, CHEN G P, journalName=Drug Stand China(中国药品标准), refType=null, unstructuredReference=ZHANG W Q, LIU Y X, CHEN G P, et al. Effect of different pretreatment methods on the detection of pesticide residues in five traditional Chinese medicines[J]. Drug Stand China(中国药品标准), 2024, 25(3):251-256., articleTitle=Effect of different pretreatment methods on the detection of pesticide residues in five traditional Chinese medicines, refAbstract=null)], funds=[Fund(id=1193712701856772535, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193674740968682493, awardId=RS2024Z006-110, language=CN, fundingSource=国家药品监督管理局药品监管科学体系建设重点项目资助(RS2024Z006-110), fundOrder=null, country=null), Fund(id=1193712701911298488, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193674740968682493, awardId=2024Z01, language=CN, fundingSource=2024年度国家药品标准制修订研究课题资助(2024Z01), fundOrder=null, country=null), Fund(id=1193712702028739001, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193674740968682493, awardId=2024ZDZ14, language=CN, fundingSource=广东省药品监督管理局科技创新项目资助(2024ZDZ14), fundOrder=null, country=null)], companyList=[AuthorCompany(id=1193712691429732727, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193674740968682493, xref=1, ext=[AuthorCompanyExt(id=1193712691438121336, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193674740968682493, companyId=1193712691429732727, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1 Key Laboratory of Traditional Chinese Medicine Quality Control and Safety Evaluation of Guangdong Provincial Drug Administration,Guangdong Institute for Drug Control, Guangzhou 510663, China), AuthorCompanyExt(id=1193712691446509945, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193674740968682493, companyId=1193712691429732727, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1 广东省药品检验所, 广东省药品监督管理局中药质量控制与安全评价重点实验室, 广州 510663)]), AuthorCompany(id=1193712691538784634, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193674740968682493, xref=2, ext=[AuthorCompanyExt(id=1193712691547173243, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193674740968682493, companyId=1193712691538784634, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=2 National Institutes for Food and Drug Control, Beijing 100050, China), AuthorCompanyExt(id=1193712691555561852, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193674740968682493, companyId=1193712691538784634, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=2 中国食品药品检定研究院, 北京 100050)]), AuthorCompany(id=1193712691664613757, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193674740968682493, xref=3, ext=[AuthorCompanyExt(id=1193712691673002366, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193674740968682493, companyId=1193712691664613757, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=3 Chinese Pharmacopoeia Commission, Beijing 100061, China), AuthorCompanyExt(id=1193712691681390975, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193674740968682493, companyId=1193712691664613757, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=3 国家药典委员会, 北京 100061)])], figs=[ArticleFig(id=1193712700439097773, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193674740968682493, language=EN, label=Tab.1, caption=

Detection parameters of pesticide residue related reference in Atractylodis Macrocephalae Rhizoma by GC-MS/MS

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No. Compound tR/min Monitored ion pairs CE/V No. Compound tR/min Monitored ion pairs CE/V
1 Metaldehyde 3.4,3.6 89.00>45.10 16 26 o,p'-DDT 22.4 235.00>165.00 16
89.00>43.00 12 235.00>199.00 10
2 Ethoprophos 8.9 200.00>158.00 12 27 p,p'-DDE 22.5 246.00>176.00 22
200.00>114.00 21 246.00>220.00 13
3 Chlordimeform 9.2 152.00>117.00 15 28 Fenamiphos 22.6 303.10>195.10 22
196.00>181.00 18 303.10>154.10 14
4 Sulfotep 9.8 322.00>202.00 22 29 Dieldrin 22.8 276.90>241.00 12
322.00>174.00 25 276.90>172.00 11
5 Phorate 10.9 260.00>75.00 13 30 Flusilazol 22.9 233.10>165.10 14
230.80>175.00 11 233.10>152.10 14
6 BHC 11.1,12.2,12.4,13.5 218.90>182.90 24 31 Phosfolan-methyl 23.1 227.00>92.00 18
218.90>111.00 22 227.00>168.00 25
7 Terbufos 11.6 231.00>174.90 15 32 Kresoxim-methyl 23.2 206.10>116.10 6
231.00>203.00 24 206.10>131.10 14
8 Pyrimethani 11.6 198.10>183.10 14 33 p,p'-DDD 23.8 235.00>165.00 15
198.10>118.10 18 235.00>199.00 16
9 Monocrotophos 12.4 127.10>109.00 15 34 Fipronil sulfone 23.8 382.95>255.00 22
127.10>95.00 20 382.95>213.00 6
10 Chlorothaloni 12.7 265.90>230.80 14 35 β-Endosulfan 24.2 338.90>160.00 25
265.90>168.00 22 206.80>171.80 20
11 Diazinon 12.7 304.10>179.10 10 36 Nitrofen 24.5 282.90>162.00 15
304.10>162.10 8 282.90>201.00 12
12 Dicofol 14.1,15.1 250.00>139.00 22 37 p,p'-DDT 24.9 235.00>165.00 17
250.00>215.00 23 235.00>199.00 25
13 Parathion-methyl 15.3 263.00>109.00 14 38 Dazomet 25 162.10>89.10 8
263.00>79.00 17 89.10>44.00 10
14 Metalaxyl 15.4 249.20>190.10 8 39 Propiconazol 25.6,25.8 259.00>69.00 14
249.20>146.10 22 259.00>173.00 8
15 Fipronil 16.4 387.95>332.90 17 40 Endosulfan sulfate 25.8 386.80>288.80 18
387.95>280.90 10 272.00>237.00 16
16 Chlorpyrifos 17.0 313.90>257.90 1 41 Tebuconazole 26.3 250.10>125.10 22
313.90>285.90 8 250.10>153.10 12
17 Aldrin 17.5 262.90>193.00 23 42 Fenpyroximate 26.4,26.5 135.10>107.10 16
262.90>203.00 12 135.10>77.00 24
18 Parathion 18.4 291.10>109.00 12 43 Coumaphos 26.5 362.00>109.00 21
291.10>81.00 22 362.00>225.00 15
19 Isocarbophos 18.6 289.10>136.00 1 44 Epoxiconazole 26.8 192.00>138.00 14
135.7>108.00 25 192.00>111.00 26
20 Cyprodini 18.8 224.10>208.10 16 45 Bifenthrin 27.6 181.10>166.10 12
224.10>197.10 22 181.10>179.10 8
21 Fipronil sulfoxide 20.4 350.95>255.00 28 46 Cyhalothrin 28.9,29.23 197.00>141.00 8
350.95>227.00 16 197.00>161.00 12
22 α-Endosulfan 20.6 194.90>160.00 47 Pyridaben 30.5 147.10>117.10 22
276.80>242.00 9 147.10>132.10 14
23 Fipronil 20.9 366.90>212.90 11 48 Boscalid 31.6 342.10>140.10 14
350.00>254.90 14 342.10>112.10 28
24 Tebuconazole 21.8 214.00>172.00 20 49 Cypermethrin 31.5,31.7,31.8,31.8 181.10>152.10 22
214.00>159.00 20 181.10>127.10 22
25 Fludioxonil 22.3 248.00>182.00 14 50 Fenvalerate 32.8,33.2 419.10>225.10 6
248.00>127.00 20 419.10>125.10 12
), ArticleFig(id=1193712700522983854, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193674740968682493, language=CN, label=表1, caption=

白术中农药残留相关对照品的气相色谱-串联质谱联用(GC-MS/MS)法检测参数

, figureFileSmall=null, figureFileBig=null, tableContent=
No. Compound tR/min Monitored ion pairs CE/V No. Compound tR/min Monitored ion pairs CE/V
1 Metaldehyde 3.4,3.6 89.00>45.10 16 26 o,p'-DDT 22.4 235.00>165.00 16
89.00>43.00 12 235.00>199.00 10
2 Ethoprophos 8.9 200.00>158.00 12 27 p,p'-DDE 22.5 246.00>176.00 22
200.00>114.00 21 246.00>220.00 13
3 Chlordimeform 9.2 152.00>117.00 15 28 Fenamiphos 22.6 303.10>195.10 22
196.00>181.00 18 303.10>154.10 14
4 Sulfotep 9.8 322.00>202.00 22 29 Dieldrin 22.8 276.90>241.00 12
322.00>174.00 25 276.90>172.00 11
5 Phorate 10.9 260.00>75.00 13 30 Flusilazol 22.9 233.10>165.10 14
230.80>175.00 11 233.10>152.10 14
6 BHC 11.1,12.2,12.4,13.5 218.90>182.90 24 31 Phosfolan-methyl 23.1 227.00>92.00 18
218.90>111.00 22 227.00>168.00 25
7 Terbufos 11.6 231.00>174.90 15 32 Kresoxim-methyl 23.2 206.10>116.10 6
231.00>203.00 24 206.10>131.10 14
8 Pyrimethani 11.6 198.10>183.10 14 33 p,p'-DDD 23.8 235.00>165.00 15
198.10>118.10 18 235.00>199.00 16
9 Monocrotophos 12.4 127.10>109.00 15 34 Fipronil sulfone 23.8 382.95>255.00 22
127.10>95.00 20 382.95>213.00 6
10 Chlorothaloni 12.7 265.90>230.80 14 35 β-Endosulfan 24.2 338.90>160.00 25
265.90>168.00 22 206.80>171.80 20
11 Diazinon 12.7 304.10>179.10 10 36 Nitrofen 24.5 282.90>162.00 15
304.10>162.10 8 282.90>201.00 12
12 Dicofol 14.1,15.1 250.00>139.00 22 37 p,p'-DDT 24.9 235.00>165.00 17
250.00>215.00 23 235.00>199.00 25
13 Parathion-methyl 15.3 263.00>109.00 14 38 Dazomet 25 162.10>89.10 8
263.00>79.00 17 89.10>44.00 10
14 Metalaxyl 15.4 249.20>190.10 8 39 Propiconazol 25.6,25.8 259.00>69.00 14
249.20>146.10 22 259.00>173.00 8
15 Fipronil 16.4 387.95>332.90 17 40 Endosulfan sulfate 25.8 386.80>288.80 18
387.95>280.90 10 272.00>237.00 16
16 Chlorpyrifos 17.0 313.90>257.90 1 41 Tebuconazole 26.3 250.10>125.10 22
313.90>285.90 8 250.10>153.10 12
17 Aldrin 17.5 262.90>193.00 23 42 Fenpyroximate 26.4,26.5 135.10>107.10 16
262.90>203.00 12 135.10>77.00 24
18 Parathion 18.4 291.10>109.00 12 43 Coumaphos 26.5 362.00>109.00 21
291.10>81.00 22 362.00>225.00 15
19 Isocarbophos 18.6 289.10>136.00 1 44 Epoxiconazole 26.8 192.00>138.00 14
135.7>108.00 25 192.00>111.00 26
20 Cyprodini 18.8 224.10>208.10 16 45 Bifenthrin 27.6 181.10>166.10 12
224.10>197.10 22 181.10>179.10 8
21 Fipronil sulfoxide 20.4 350.95>255.00 28 46 Cyhalothrin 28.9,29.23 197.00>141.00 8
350.95>227.00 16 197.00>161.00 12
22 α-Endosulfan 20.6 194.90>160.00 47 Pyridaben 30.5 147.10>117.10 22
276.80>242.00 9 147.10>132.10 14
23 Fipronil 20.9 366.90>212.90 11 48 Boscalid 31.6 342.10>140.10 14
350.00>254.90 14 342.10>112.10 28
24 Tebuconazole 21.8 214.00>172.00 20 49 Cypermethrin 31.5,31.7,31.8,31.8 181.10>152.10 22
214.00>159.00 20 181.10>127.10 22
25 Fludioxonil 22.3 248.00>182.00 14 50 Fenvalerate 32.8,33.2 419.10>225.10 6
248.00>127.00 20 419.10>125.10 12
), ArticleFig(id=1193712700611064239, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193674740968682493, language=EN, label=Tab.2, caption=

Detection of mobile phase gradient elution conditions of pesticide residue related reference in Atractylodis Macrocephalae Rhizoma by LC-MS/MS

, figureFileSmall=null, figureFileBig=null, tableContent=
t/min Mobile phase A/% Mobile phase B/%
0 -1 95 5
1 -4 95→40 5→60
4 -8 40→36 60→64
8 -8.5 36→32 64→68
8.5 -9 32→25 68→75
9 -16 25→5 75→95
16 -20 5 95
20 -20.1 5→95 95→5
20.1 -25 95 5
), ArticleFig(id=1193712700673978800, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193674740968682493, language=CN, label=表2, caption=

白术中农药残留相关对照品的液相色谱-串联质谱联用(LC-MS/MS)法检测流动相洗脱条件

, figureFileSmall=null, figureFileBig=null, tableContent=
t/min Mobile phase A/% Mobile phase B/%
0 -1 95 5
1 -4 95→40 5→60
4 -8 40→36 60→64
8 -8.5 36→32 64→68
8.5 -9 32→25 68→75
9 -16 25→5 75→95
16 -20 5 95
20 -20.1 5→95 95→5
20.1 -25 95 5
), ArticleFig(id=1193712700732699057, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193674740968682493, language=EN, label=Tab.3, caption=

Detection parameters of pesticide residue related reference in Atractylodis Macrocephalae Rhizoma by LC-MS/MS

, figureFileSmall=null, figureFileBig=null, tableContent=
No. Compound tR/min Monitored ion pairs CE/V No. Compound tR/min Monitored ion pairs CE/V
1 Propamocarb 5.2 189.1>102.0 17 38 Abamectin 18.1 890.6>305.2 30
189.1>144.0 12 890.6>567.4 25
2 Carbendazim 6.3 192.1>132.1 28 39 Fludioxonil 11.4 246.9>126.0 30
192.1>160.1 18 246.9>168.9 35
3 Pyrimethani 11.2 200.0>82.0 24 40 Hymexazol 4.2 100.0>54.1 8
200.0>107.0 24 100.0>44.1 9
4 Pymetrozine 5.3 218.0>79.0 30 41 Iprodione 12.2 330.1>244.9 20
218.0>105.0 20 330.1>247.0 21
5 Acetamiprid 6.3 223.0>56.1 15 42 Clothianidin 5.5 250.0>169.1 17
223.0>126.0 20 250.0>132.0 21
6 Cyprodini 13.3 226.0>93.0 33 43 Methamidophos 4.1 142.1>93.9 16
226.0>108.0 25 142.1>125.0 21
7 Imidacloprid 6.1 256.1>175.1 20 44 Chlordimeform 5.9 197.1>46.1 20
256.1>209.1 15 197.1>117.1 22
8 Metalaxyl 9.5 280.1>192.1 17 45 Aldicarb sulfoxide 5.0 207.2> 132.1 13
280.1>220.1 13 207.2>89.2 16
9 Tridemorph 13.9 298.2>130.1 25 46 Aldicarb 7.0 213.1>89.1 17
298.2>116.3 25 213.1>116.2 24
10 Diazinon 13.5 305.1>96.9 35 47 Carbofuran 7.7 222.1> 165.1 27
305.1>169.0 22 222.1> 123.1 13
11 Tebuconazole 13.4 308.0>125.0 22 48 Aldicarb sulfone 5.2 223.1>86.2 18
308.0>70.1 40 223.1>223.1 15
12 Hexaconazole 13.9 314.0>70.1 22 49 Monocrotophos 5.7 224.1 > 127.1 22
314.0>159.0 28 224.1 > 193.1 20
13 Kresoxim-methyl 13.1 314.1>206.0 12 50 Carbofuran-3-hydroxy 6.2 238.2>181.1 13
314.1>116.0 7 238.2>183.3 18
14 Flusilazol 12.8 316.0>247.0 28 51 Ethoprophos 12.3 243.2>131.1 22
316.0>165.0 18 243.2>97.0 30
15 Pyrethrins Ⅰ 16.7 328.9>161.2 15 52 Fonofos 13.3 247.1>109.1 26
328.9>143.0 10 247.1>137.1 17
16 Pyrethrins Ⅱ 14.3 328.9>161.2 15 53 Phosfolan 6.8 256.1>140.0 25
328.9>143.0 10 256.1>168.0 25
17 Epoxiconazole 12.5 329.9>121.1 20 54 Demeton 10.6 259.1>89.0 14
329.9>141.0 15 259.1>61.0 30
18 Propiconazol 13.5 342.0>159.0 22 55 Phorate 13.8 261.0>75.0 20
342.0>69.0 34 261.0>47.0 30
19 Boscalid 11.4 342.9>307.0 20 56 Posfolan-methyl 17.2 228.0>168.0 23
342.9>139.9 20 228.0>109.0 25
20 Chlorpyrifos 16.1 349.5>97.0 25 57 Cadusafos 14.2 271.0>131.0 22
349.5>198.0 25 271.0>97.0 20
21 Tebufenozide 12.8 353.1>297.1 20 58 Phorate sulfoxide 8.7 277.0>171.0 15
353.1>133.0 8 277.0>199.0 20
22 Pyridaben 17.5 365.1>309.1 24 59 Isocarbophos 9.5 312.0>270.0 18
365.1>147.1 12 312.0>236.0 22
23 Propargite 16.5 368.0>175.0 30 60 Phorate sulfone 8.9 293.0>247.0 15
368.0>231.1 20 293.0>115.0 22
24 Flumorph 16.3 372.0>268.0 20 61 Phosphamidon 7.1 300.0>174.0 24
372.0>165.1 20 300.0>127.0 24
25 Spirotetramat 12.2 374.1>172.2 30 62 Fenamiphos 12.7 304.0>217.0 27
374.1>330.1 15 304.0>202.0 24
26 Prochloraz 13.9 376.0>70.1 34 63 Terbufos sulfoxide 10.7 305.0>186.9 25
376.0>307.1 16 305.0>97.0 25
27 Pyraclostrobin 13.7 388.1>193.9 25 64 Isazafos 11.8 314.0>161.9 25
388.1>163 12 314.0>120.0 18
28 Dimethomorph 11.6 388.1>300.9 30 65 Fenamiphos sulfoxide 7.5 320.0>233.2 28
388.1>165.3 20 320.0>171.3 28
29 Difenoconazole 14.3 406.1>251.1 60 66 Terbufos sulfone 17.8 321.0>171.2 26
406.1>111.1 25 321.0>97.2 28
30 Mandipropamid 11.4 412.3>356.2 16 67 Sulfotep 13.0 323.0>97.0 18
412.3>328.2 10 323.0>115.0 20
31 Pyraoxystrobin 13.7 413.1>205.0 8 68 Isofenphos-methyl 12.9 332.3>273.1 15
413.1>172.9 15 332.3>231.1 15
32 Fenpyroximate 16.8 422.2>366.1 32 69 Fenamiphos sulfone 7.7 336.0>266.0 25
422.2>138.1 15 336.0>188.0 25
33 Fluazinam 19.3 466.1>329.1 15 70 Chlorsulfuron 7.5 358.0>141.0 27
466.1>175.0 15 358.0>167.0 27
34 Validamycin 1.7 498.1>178.0 30 71 Coumaphos 13.4 363.0>227.0 25
498.1>142.0 30 363.0>307.0 25
35 Thifluzamide 12.5 528.6>147.7 35 72 Metsulfuron-methyl 7.2 382.0>167.0 22
528.6>508.6 25 382.0>199.0 22
36 Spinetoram 14.9 749.0>98.0 30 73 Ethametsulfuron-methyl 8.2 411.0>196.0 15
749.0>141.1 30 411.0>168.0 15
37 Emamectin benzoate 16.0 886.6>157.7 40
886.6>302.1 35
), ArticleFig(id=1193712700816585138, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193674740968682493, language=CN, label=表3, caption=

白术中农药残留相关对照品的LC-MS/MS法检测参数

, figureFileSmall=null, figureFileBig=null, tableContent=
No. Compound tR/min Monitored ion pairs CE/V No. Compound tR/min Monitored ion pairs CE/V
1 Propamocarb 5.2 189.1>102.0 17 38 Abamectin 18.1 890.6>305.2 30
189.1>144.0 12 890.6>567.4 25
2 Carbendazim 6.3 192.1>132.1 28 39 Fludioxonil 11.4 246.9>126.0 30
192.1>160.1 18 246.9>168.9 35
3 Pyrimethani 11.2 200.0>82.0 24 40 Hymexazol 4.2 100.0>54.1 8
200.0>107.0 24 100.0>44.1 9
4 Pymetrozine 5.3 218.0>79.0 30 41 Iprodione 12.2 330.1>244.9 20
218.0>105.0 20 330.1>247.0 21
5 Acetamiprid 6.3 223.0>56.1 15 42 Clothianidin 5.5 250.0>169.1 17
223.0>126.0 20 250.0>132.0 21
6 Cyprodini 13.3 226.0>93.0 33 43 Methamidophos 4.1 142.1>93.9 16
226.0>108.0 25 142.1>125.0 21
7 Imidacloprid 6.1 256.1>175.1 20 44 Chlordimeform 5.9 197.1>46.1 20
256.1>209.1 15 197.1>117.1 22
8 Metalaxyl 9.5 280.1>192.1 17 45 Aldicarb sulfoxide 5.0 207.2> 132.1 13
280.1>220.1 13 207.2>89.2 16
9 Tridemorph 13.9 298.2>130.1 25 46 Aldicarb 7.0 213.1>89.1 17
298.2>116.3 25 213.1>116.2 24
10 Diazinon 13.5 305.1>96.9 35 47 Carbofuran 7.7 222.1> 165.1 27
305.1>169.0 22 222.1> 123.1 13
11 Tebuconazole 13.4 308.0>125.0 22 48 Aldicarb sulfone 5.2 223.1>86.2 18
308.0>70.1 40 223.1>223.1 15
12 Hexaconazole 13.9 314.0>70.1 22 49 Monocrotophos 5.7 224.1 > 127.1 22
314.0>159.0 28 224.1 > 193.1 20
13 Kresoxim-methyl 13.1 314.1>206.0 12 50 Carbofuran-3-hydroxy 6.2 238.2>181.1 13
314.1>116.0 7 238.2>183.3 18
14 Flusilazol 12.8 316.0>247.0 28 51 Ethoprophos 12.3 243.2>131.1 22
316.0>165.0 18 243.2>97.0 30
15 Pyrethrins Ⅰ 16.7 328.9>161.2 15 52 Fonofos 13.3 247.1>109.1 26
328.9>143.0 10 247.1>137.1 17
16 Pyrethrins Ⅱ 14.3 328.9>161.2 15 53 Phosfolan 6.8 256.1>140.0 25
328.9>143.0 10 256.1>168.0 25
17 Epoxiconazole 12.5 329.9>121.1 20 54 Demeton 10.6 259.1>89.0 14
329.9>141.0 15 259.1>61.0 30
18 Propiconazol 13.5 342.0>159.0 22 55 Phorate 13.8 261.0>75.0 20
342.0>69.0 34 261.0>47.0 30
19 Boscalid 11.4 342.9>307.0 20 56 Posfolan-methyl 17.2 228.0>168.0 23
342.9>139.9 20 228.0>109.0 25
20 Chlorpyrifos 16.1 349.5>97.0 25 57 Cadusafos 14.2 271.0>131.0 22
349.5>198.0 25 271.0>97.0 20
21 Tebufenozide 12.8 353.1>297.1 20 58 Phorate sulfoxide 8.7 277.0>171.0 15
353.1>133.0 8 277.0>199.0 20
22 Pyridaben 17.5 365.1>309.1 24 59 Isocarbophos 9.5 312.0>270.0 18
365.1>147.1 12 312.0>236.0 22
23 Propargite 16.5 368.0>175.0 30 60 Phorate sulfone 8.9 293.0>247.0 15
368.0>231.1 20 293.0>115.0 22
24 Flumorph 16.3 372.0>268.0 20 61 Phosphamidon 7.1 300.0>174.0 24
372.0>165.1 20 300.0>127.0 24
25 Spirotetramat 12.2 374.1>172.2 30 62 Fenamiphos 12.7 304.0>217.0 27
374.1>330.1 15 304.0>202.0 24
26 Prochloraz 13.9 376.0>70.1 34 63 Terbufos sulfoxide 10.7 305.0>186.9 25
376.0>307.1 16 305.0>97.0 25
27 Pyraclostrobin 13.7 388.1>193.9 25 64 Isazafos 11.8 314.0>161.9 25
388.1>163 12 314.0>120.0 18
28 Dimethomorph 11.6 388.1>300.9 30 65 Fenamiphos sulfoxide 7.5 320.0>233.2 28
388.1>165.3 20 320.0>171.3 28
29 Difenoconazole 14.3 406.1>251.1 60 66 Terbufos sulfone 17.8 321.0>171.2 26
406.1>111.1 25 321.0>97.2 28
30 Mandipropamid 11.4 412.3>356.2 16 67 Sulfotep 13.0 323.0>97.0 18
412.3>328.2 10 323.0>115.0 20
31 Pyraoxystrobin 13.7 413.1>205.0 8 68 Isofenphos-methyl 12.9 332.3>273.1 15
413.1>172.9 15 332.3>231.1 15
32 Fenpyroximate 16.8 422.2>366.1 32 69 Fenamiphos sulfone 7.7 336.0>266.0 25
422.2>138.1 15 336.0>188.0 25
33 Fluazinam 19.3 466.1>329.1 15 70 Chlorsulfuron 7.5 358.0>141.0 27
466.1>175.0 15 358.0>167.0 27
34 Validamycin 1.7 498.1>178.0 30 71 Coumaphos 13.4 363.0>227.0 25
498.1>142.0 30 363.0>307.0 25
35 Thifluzamide 12.5 528.6>147.7 35 72 Metsulfuron-methyl 7.2 382.0>167.0 22
528.6>508.6 25 382.0>199.0 22
36 Spinetoram 14.9 749.0>98.0 30 73 Ethametsulfuron-methyl 8.2 411.0>196.0 15
749.0>141.1 30 411.0>168.0 15
37 Emamectin benzoate 16.0 886.6>157.7 40
886.6>302.1 35
), ArticleFig(id=1193712700896276915, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193674740968682493, language=EN, label=null, caption=null, figureFileSmall=null, figureFileBig=null, tableContent=
No. Pesticide
indicators		 Linear
equation		 r Linearity range
/ng·mL-1		 Average
recovery/%		 RSD/%
Repeatability Precision
1 Metaldehyde y=608.7x-959.3 0.999 4 1 -400 101.0 7.6 6.6
2 Phorate y=1 216.1x +556.6 0.999 6 1 -100 109.7 6.6 5.7
3 BHC y=935.14x-304.0 0.999 5 0.4 -40 77.7 6.4 4.5
4 Terbufos y=432.8x +525.9 0.999 9 0.4 -40 99.9 6.6 5.6
5 Chlorothaloni y=270.3x-5487.8 0.998 6 10 -400 106.8 9.0 6.6
6 Dicofol y=1 267.2x +1 644.6 0.999 8 1 -50 102.3 7.6 5.0
7 Parathion-methyl y=2 107.3x-960.4 0.999 6 4 -40 100.6 5.1 2.3
8 Fipronil y=384.0x +1 021.6 0.999 5 1 -100 96.9 6.4 8.0
9 Chlorpyrifos y=623.1x-3 409.1 0.998 4 1 -400 100.9 5.7 2.7
10 Aldrin y=503.7x +1 760.1 0.999 7 1 -100 100.5 4.7 5.9
11 Parathion y=1 932.1x +678.5 0.999 8 1 -50 100.8 4.3 2.1
12 Fipronil sulfoxide y=654.5x +635.2 0.999 5 4 -400 96.9 3.6 3.0
13 α-Endosulfan y=330.2x-3 075.6 0.999 6 4 -400 99.6 6.4 10.8
14 Fipronil y=2 447.8x +1 119.2 0.998 9 4 -400 94.4 5.4 5.4
15 o,p'-DDT y=667.3x-2 229.7 0.999 9 1 -100 102.0 4.0 5.7
16 p,p'-DDE y=1 855.0x +2 809.5 0.999 6 1 -100 97.6 6.3 2.7
17 Dieldrin y=110.7x +931.8 0.999 6 1 -100 98.0 2.5 3.4
18 Kresoxim-methyl y=1 078.1x +337.6 0.999 8 1 -100 100.3 6.3 5.0
19 Kresoxim-methyl y=492.6x-1 840.6 0.998 7 1 -200 96.8 5.9 6.4
20 p,p'-DDD y=1 658.7x-490.9 0.999 5 1 -100 97.6 2.9 1.9
21 Fipronil sulfone y=386.7x +241.9 0.999 8 1 -100 102.4 4.4 4.1
22 β-Endosulfan y=311.2x +200.0 0.999 6 1 -100 89.7 5.2 9.6
23 Nitrofen y=1 841.7x-346.6 0.999 9 1 -100 94.9 2.0 2.6
24 p,p'-DDT y=8 989.2x-3 018.0 0.999 8 1 -100 122.9 6.5 3.1
25 Dazomet y=538.1x-311.0 0.998 5 10 -200 95.6 0.8 2.0
26 Endosulfan sulfate y=539.7x-801.7 0.999 3 1 -100 94.2 6.1 7.4
27 Bifenthrin y=12 212.4x-60 007.1 0.998 7 1 -400 92.8 7.8 2.9
28 Cyhalothrin y=493.2x-731.0 0.998 8 1 -100 99.6 1.9 3.4
29 Cypermethrin y=341.8x-955.5 0.998 8 1 -200 116.0 7.2 5.7
30 Fenvalerate y=53.7x-1 404.1 0.993 8 10 -400 87.2 6.8 4.9
31 Propamocarb y=68 223.1x-15 414 0.995 3 1 -100 96.2 1.1 1.7
32 Carbendazim y=26 241.3x-639.243 0.995 9 1 -100 101.9 2.8 4.7
33 Pyrimethanil y=6 584.18x-1 320.35 0.997 3 1 -100 107.0 3.0 3.1
34 Pymetrozin y=7 493.23x+364.189 0.998 1 1 -100 94.2 4.1 2.8
35 Acetamiprid y=44 497.5x+7 121.96 0.997 9 1 -100 100.5 4.3 7.6
36 Cyprodinil y=10 559.4x+1 038.25 0.996 1 -100 94.8 3.8 8.5
37 Imidacloprid y=34 929x+5 173.62 0.998 6 1 -100 95.3 7.6 5.8
38 Metalaxyl y=85 530.3x-2 760.97 0.997 6 1 -100 84.2 6.1 7.8
39 Tridemorph y=30 315.2x+24 155.3 0.991 5 1 -100 101.4 7.4 5.8
40 Diazinon y=74 776x+5 730.01 0.998 1 1 -100 97.0 7.8 4.7
41 Tebuconazole y=5 865.71x+2 709.57 0.997 7 1 -100 89.1 7.1 7.8
42 Hexaconazole y=35 174.8x+8 650.65 0.998 4 1 -100 99.7 6.2 7.8
43 Flusilazole y=70 780.4x+26 471.4 0.999 2 1 -100 89.7 6.6 2.9
44 Pyrethrin Ⅰ y=1 495.5x +905.3 0.999 9 1 -40 107.8 3.2 4.9
45 Pyrethrin Ⅱ y=1 531.9x-466.2 0.997 8 1 -60 85.7 5.9 3.7
46 Epoxiconazole y=90 975.5x+27 766.8 0.998 8 1 -100 91.4 3.3 3.9
47 Propiconazole y=39 323.5x+17 163.3 0.998 2 1 -100 86.6 4.9 3.0
48 Boscalid y=48 486.8x+4 993.18 0.997 8 1 -100 77.8 6.5 2.8
49 Tebufenozide y=4 887.42x+506.746 0.997 9 1 -100 113.7 2.9 7.7
50 Pyridaben y=33 406.9x+140 274 0.989 8 1 -100 69.5 4.0 2.8
51 Propargite y=14 129.3x+66 066.6 0.992 2 1 -100 93.4 3.4 5.0
52 Flumorph y=18 832.3x-10 316.8 0.999 5 1 -400 98.7 1.8 3.3
53 Spirotetramat y=62 488.1x-2 432.01 0.998 1 -100 99.0 6.2 2.7
54 Prochloraz y=7 402.86x+13 091.1 0.997 5 1 -100 54.7 1.1 8.0
55 Pyraclostrobin y=69 111.2x+112 625 0.996 5 1 -100 104.2 7.7 2.2
56 Dimethomorph y=109 969x-1 509.79 0.998 2 1 -100 76.7 7.2 7.9
57 Difenoconazole y=75 436.9x+120 102 0.997 4 1 -100 92.8 2.6 7.7
58 Mandipropamid y=32 170.6x+9 161.1 0.997 8 1 -100 82.8 1.5 3.4
59 Pyraoxystrobin y=95 618.2x+121 505 0.999 1 1 -100 69.0 2.1 4.7
60 Fenpyroximate y=82 534.9x+277 846 0.994 1 1 -100 98.8 2.8 1.8
61 Fluazinam y=24 384.0x+1 134.3 0.997 8 1 -100 84.4 4.7 5.8
62 Validamycin y=7 130.4.0x-238.4 0.999 5 2 -200 78.0 2.5 5.6
63 Thifluzamide y=20 742.4x+546.199 0.998 1 1 -100 99.8 6.9 2.1
64 Pyrimethanil y=2 190.44x+289.637 0.997 5 1 -100 90.1 6.4 8.5
65 Emamectin benzoate y=69 124.1x+5 909.56 0.997 9 1 -100 79.9 1.8 1.3
66 Abamectin y=914.613x+813.745 0.997 6 1 -100 78.7 1.7 2.4
67 Fludioxonil y=32.480 4x-1 010.23 0.99 25 -400 93.7 7.0 5.4
68 Hymexazol y=27 233.5x-6 074.88 0.995 4 1 -100 102.3 2.5 3.4
69 Iprodione y=256 208x+39 674.9 0.999 7 1 -25 81.9 3.9 5.3
70 Clothianidin y=7 589.23x+14 658.3 0.99 7 1 -100 85.6 3.0 1.3
71 Methamidophos y=14 781.1x+1 042.29 0.998 8 1 -50 78.7 2.8 2.4
72 Chlordimeform y=14 466.8x-6 163.11 0.998 1 1 -50 74.7 2.0 1.6
73 Aldicarb sulfoxide y=13 508x-16 436.5 0.996 6 1 -50 93.0 4.1 6.6
74 Aldicarb y=15.620 1x-92.366 4 0.998 1 -50 83.0 4.8 5.8
75 Carbofuran y=11 348.7x-2 434.64 0.999 6 1 -50 111.4 3.7 7.6
76 Aldicarb sulfone y=1 015.54x-812.087 0.996 3 20 -100 80.6 5.0 2.2
77 Monocrotophos y=31 639.6x-3 633.91 0.998 7 0.6 -30 85.9 19.1 4.2
78 Carbofuran-3-hydroxy y=48 669.3x-19 174.8 0.998 7 1 -50 78.6 20.7 2.2
79 Ethoprophos y=18 971.1x-1 703.21 0.999 6 0.4 -20 96.3 18.4 2.1
80 Fonofos y=3 596.38x-491.188 0.999 8 0.4 -20 113.4 10.3 7.0
81 Phosfolan y=226 860x-11 341.1 0.999 9 0.6 -30 95.2 2.3 2.2
82 Demeton y=112.817x-41.812 1 0.999 6 8 -40 88.8 7.4 2.6
83 Cadusafos y=65 200x+4 089 0.999 8 0.4 -20 79.8 2.8 0.7
84 Phorate sulfoxide y=31 521.4x-4 244.62 0.999 9 1 -50 88.7 1.8 3.4
85 Isocarbophos y=26 222.8x+4 997.45 0.999 2 1 -50 69.1 6.5 1.6
86 Phorate sulfone y=2 511.44x-886.691 0.992 0.4 -20 79.4 4.8 1.9
87 Phosphamidon y=63 359.8x-29 401.9 0.998 3 1 -50 75.5 6.4 4.1
88 Fenamiphos y=108 105x-3 407.72 0.999 9 0.4 -20 84.5 4.5 6.3
89 Terbufos sulfoxide y=4 366.99x-936.447 0.997 4 0.4 -20 81.9 20.0 2.6
90 Isazafos y=59 621.2x+4 671.58 0.999 7 0.2 -10 90.9 1.4 2.6
91 Terbufos sulfone y=26 426.3x-33 388.8 0.997 3 0.4 -20 75.5 1.7 4.8
92 Terbufos sulfoxide y=1 155.43x+525.341 0.999 2 0.4 -20 97.3 8.6 2.3
93 Sulfotep y=35 029.6x-10 803.9 0.998 4 0.4 -20 106.7 4.4 3.7
94 Isofenphos-methyl y=544.14x-589.019 0.998 2 0.4 -20 91.8 3.3 4.6
95 Fenamiphos sulfone y=33 635.2x-14 919.2 0.999 0.4 -20 75.6 2.7 6.2
96 Chlorsulfuron y=20 403.8x+83 573.3 0.999 9 1 -50 67.0 16.6 2.1
97 Coumaphos y=15 800.6x-4 228.66 0.998 2 1 -50 71.0 14.4 2.2
98 Metsulfuron-methyl y=154 367x-123 197 0.998 3 1 -50 64.8 1.1 2.0
99 Ethametsulfuron-methyl y=95 410.6x-74 316 0.995 1 1 -50 62.9 2.5 1.3
), ArticleFig(id=1193712700984357300, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193674740968682493, language=CN, label=表4, caption=

白术中99种农药线性范围、r、重复性、加标回收、精密性测定结果 Tabl.4 The results of linearity range, r, repeatability, spike recovery and precision of 99 pesticides in Atractylodis Macrocephalae Rhizoma

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No. Pesticide
indicators		 Linear
equation		 r Linearity range
/ng·mL-1		 Average
recovery/%		 RSD/%
Repeatability Precision
1 Metaldehyde y=608.7x-959.3 0.999 4 1 -400 101.0 7.6 6.6
2 Phorate y=1 216.1x +556.6 0.999 6 1 -100 109.7 6.6 5.7
3 BHC y=935.14x-304.0 0.999 5 0.4 -40 77.7 6.4 4.5
4 Terbufos y=432.8x +525.9 0.999 9 0.4 -40 99.9 6.6 5.6
5 Chlorothaloni y=270.3x-5487.8 0.998 6 10 -400 106.8 9.0 6.6
6 Dicofol y=1 267.2x +1 644.6 0.999 8 1 -50 102.3 7.6 5.0
7 Parathion-methyl y=2 107.3x-960.4 0.999 6 4 -40 100.6 5.1 2.3
8 Fipronil y=384.0x +1 021.6 0.999 5 1 -100 96.9 6.4 8.0
9 Chlorpyrifos y=623.1x-3 409.1 0.998 4 1 -400 100.9 5.7 2.7
10 Aldrin y=503.7x +1 760.1 0.999 7 1 -100 100.5 4.7 5.9
11 Parathion y=1 932.1x +678.5 0.999 8 1 -50 100.8 4.3 2.1
12 Fipronil sulfoxide y=654.5x +635.2 0.999 5 4 -400 96.9 3.6 3.0
13 α-Endosulfan y=330.2x-3 075.6 0.999 6 4 -400 99.6 6.4 10.8
14 Fipronil y=2 447.8x +1 119.2 0.998 9 4 -400 94.4 5.4 5.4
15 o,p'-DDT y=667.3x-2 229.7 0.999 9 1 -100 102.0 4.0 5.7
16 p,p'-DDE y=1 855.0x +2 809.5 0.999 6 1 -100 97.6 6.3 2.7
17 Dieldrin y=110.7x +931.8 0.999 6 1 -100 98.0 2.5 3.4
18 Kresoxim-methyl y=1 078.1x +337.6 0.999 8 1 -100 100.3 6.3 5.0
19 Kresoxim-methyl y=492.6x-1 840.6 0.998 7 1 -200 96.8 5.9 6.4
20 p,p'-DDD y=1 658.7x-490.9 0.999 5 1 -100 97.6 2.9 1.9
21 Fipronil sulfone y=386.7x +241.9 0.999 8 1 -100 102.4 4.4 4.1
22 β-Endosulfan y=311.2x +200.0 0.999 6 1 -100 89.7 5.2 9.6
23 Nitrofen y=1 841.7x-346.6 0.999 9 1 -100 94.9 2.0 2.6
24 p,p'-DDT y=8 989.2x-3 018.0 0.999 8 1 -100 122.9 6.5 3.1
25 Dazomet y=538.1x-311.0 0.998 5 10 -200 95.6 0.8 2.0
26 Endosulfan sulfate y=539.7x-801.7 0.999 3 1 -100 94.2 6.1 7.4
27 Bifenthrin y=12 212.4x-60 007.1 0.998 7 1 -400 92.8 7.8 2.9
28 Cyhalothrin y=493.2x-731.0 0.998 8 1 -100 99.6 1.9 3.4
29 Cypermethrin y=341.8x-955.5 0.998 8 1 -200 116.0 7.2 5.7
30 Fenvalerate y=53.7x-1 404.1 0.993 8 10 -400 87.2 6.8 4.9
31 Propamocarb y=68 223.1x-15 414 0.995 3 1 -100 96.2 1.1 1.7
32 Carbendazim y=26 241.3x-639.243 0.995 9 1 -100 101.9 2.8 4.7
33 Pyrimethanil y=6 584.18x-1 320.35 0.997 3 1 -100 107.0 3.0 3.1
34 Pymetrozin y=7 493.23x+364.189 0.998 1 1 -100 94.2 4.1 2.8
35 Acetamiprid y=44 497.5x+7 121.96 0.997 9 1 -100 100.5 4.3 7.6
36 Cyprodinil y=10 559.4x+1 038.25 0.996 1 -100 94.8 3.8 8.5
37 Imidacloprid y=34 929x+5 173.62 0.998 6 1 -100 95.3 7.6 5.8
38 Metalaxyl y=85 530.3x-2 760.97 0.997 6 1 -100 84.2 6.1 7.8
39 Tridemorph y=30 315.2x+24 155.3 0.991 5 1 -100 101.4 7.4 5.8
40 Diazinon y=74 776x+5 730.01 0.998 1 1 -100 97.0 7.8 4.7
41 Tebuconazole y=5 865.71x+2 709.57 0.997 7 1 -100 89.1 7.1 7.8
42 Hexaconazole y=35 174.8x+8 650.65 0.998 4 1 -100 99.7 6.2 7.8
43 Flusilazole y=70 780.4x+26 471.4 0.999 2 1 -100 89.7 6.6 2.9
44 Pyrethrin Ⅰ y=1 495.5x +905.3 0.999 9 1 -40 107.8 3.2 4.9
45 Pyrethrin Ⅱ y=1 531.9x-466.2 0.997 8 1 -60 85.7 5.9 3.7
46 Epoxiconazole y=90 975.5x+27 766.8 0.998 8 1 -100 91.4 3.3 3.9
47 Propiconazole y=39 323.5x+17 163.3 0.998 2 1 -100 86.6 4.9 3.0
48 Boscalid y=48 486.8x+4 993.18 0.997 8 1 -100 77.8 6.5 2.8
49 Tebufenozide y=4 887.42x+506.746 0.997 9 1 -100 113.7 2.9 7.7
50 Pyridaben y=33 406.9x+140 274 0.989 8 1 -100 69.5 4.0 2.8
51 Propargite y=14 129.3x+66 066.6 0.992 2 1 -100 93.4 3.4 5.0
52 Flumorph y=18 832.3x-10 316.8 0.999 5 1 -400 98.7 1.8 3.3
53 Spirotetramat y=62 488.1x-2 432.01 0.998 1 -100 99.0 6.2 2.7
54 Prochloraz y=7 402.86x+13 091.1 0.997 5 1 -100 54.7 1.1 8.0
55 Pyraclostrobin y=69 111.2x+112 625 0.996 5 1 -100 104.2 7.7 2.2
56 Dimethomorph y=109 969x-1 509.79 0.998 2 1 -100 76.7 7.2 7.9
57 Difenoconazole y=75 436.9x+120 102 0.997 4 1 -100 92.8 2.6 7.7
58 Mandipropamid y=32 170.6x+9 161.1 0.997 8 1 -100 82.8 1.5 3.4
59 Pyraoxystrobin y=95 618.2x+121 505 0.999 1 1 -100 69.0 2.1 4.7
60 Fenpyroximate y=82 534.9x+277 846 0.994 1 1 -100 98.8 2.8 1.8
61 Fluazinam y=24 384.0x+1 134.3 0.997 8 1 -100 84.4 4.7 5.8
62 Validamycin y=7 130.4.0x-238.4 0.999 5 2 -200 78.0 2.5 5.6
63 Thifluzamide y=20 742.4x+546.199 0.998 1 1 -100 99.8 6.9 2.1
64 Pyrimethanil y=2 190.44x+289.637 0.997 5 1 -100 90.1 6.4 8.5
65 Emamectin benzoate y=69 124.1x+5 909.56 0.997 9 1 -100 79.9 1.8 1.3
66 Abamectin y=914.613x+813.745 0.997 6 1 -100 78.7 1.7 2.4
67 Fludioxonil y=32.480 4x-1 010.23 0.99 25 -400 93.7 7.0 5.4
68 Hymexazol y=27 233.5x-6 074.88 0.995 4 1 -100 102.3 2.5 3.4
69 Iprodione y=256 208x+39 674.9 0.999 7 1 -25 81.9 3.9 5.3
70 Clothianidin y=7 589.23x+14 658.3 0.99 7 1 -100 85.6 3.0 1.3
71 Methamidophos y=14 781.1x+1 042.29 0.998 8 1 -50 78.7 2.8 2.4
72 Chlordimeform y=14 466.8x-6 163.11 0.998 1 1 -50 74.7 2.0 1.6
73 Aldicarb sulfoxide y=13 508x-16 436.5 0.996 6 1 -50 93.0 4.1 6.6
74 Aldicarb y=15.620 1x-92.366 4 0.998 1 -50 83.0 4.8 5.8
75 Carbofuran y=11 348.7x-2 434.64 0.999 6 1 -50 111.4 3.7 7.6
76 Aldicarb sulfone y=1 015.54x-812.087 0.996 3 20 -100 80.6 5.0 2.2
77 Monocrotophos y=31 639.6x-3 633.91 0.998 7 0.6 -30 85.9 19.1 4.2
78 Carbofuran-3-hydroxy y=48 669.3x-19 174.8 0.998 7 1 -50 78.6 20.7 2.2
79 Ethoprophos y=18 971.1x-1 703.21 0.999 6 0.4 -20 96.3 18.4 2.1
80 Fonofos y=3 596.38x-491.188 0.999 8 0.4 -20 113.4 10.3 7.0
81 Phosfolan y=226 860x-11 341.1 0.999 9 0.6 -30 95.2 2.3 2.2
82 Demeton y=112.817x-41.812 1 0.999 6 8 -40 88.8 7.4 2.6
83 Cadusafos y=65 200x+4 089 0.999 8 0.4 -20 79.8 2.8 0.7
84 Phorate sulfoxide y=31 521.4x-4 244.62 0.999 9 1 -50 88.7 1.8 3.4
85 Isocarbophos y=26 222.8x+4 997.45 0.999 2 1 -50 69.1 6.5 1.6
86 Phorate sulfone y=2 511.44x-886.691 0.992 0.4 -20 79.4 4.8 1.9
87 Phosphamidon y=63 359.8x-29 401.9 0.998 3 1 -50 75.5 6.4 4.1
88 Fenamiphos y=108 105x-3 407.72 0.999 9 0.4 -20 84.5 4.5 6.3
89 Terbufos sulfoxide y=4 366.99x-936.447 0.997 4 0.4 -20 81.9 20.0 2.6
90 Isazafos y=59 621.2x+4 671.58 0.999 7 0.2 -10 90.9 1.4 2.6
91 Terbufos sulfone y=26 426.3x-33 388.8 0.997 3 0.4 -20 75.5 1.7 4.8
92 Terbufos sulfoxide y=1 155.43x+525.341 0.999 2 0.4 -20 97.3 8.6 2.3
93 Sulfotep y=35 029.6x-10 803.9 0.998 4 0.4 -20 106.7 4.4 3.7
94 Isofenphos-methyl y=544.14x-589.019 0.998 2 0.4 -20 91.8 3.3 4.6
95 Fenamiphos sulfone y=33 635.2x-14 919.2 0.999 0.4 -20 75.6 2.7 6.2
96 Chlorsulfuron y=20 403.8x+83 573.3 0.999 9 1 -50 67.0 16.6 2.1
97 Coumaphos y=15 800.6x-4 228.66 0.998 2 1 -50 71.0 14.4 2.2
98 Metsulfuron-methyl y=154 367x-123 197 0.998 3 1 -50 64.8 1.1 2.0
99 Ethametsulfuron-methyl y=95 410.6x-74 316 0.995 1 1 -50 62.9 2.5 1.3
), ArticleFig(id=1193712701080826293, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1193674740968682493, language=EN, label=Tab.5, caption=

Pesticide determination results of 53 batches of Atractylodis Macrocephalae Rhizoma samples

, figureFileSmall=null, figureFileBig=null, tableContent=
No. Pesticide indicator ADI/mg·kg-1 bw Detection rate /% Residual amount/mg·kg-1 Registration status HQc [12]
1 Tebuconazole 0.03 100.0 0.06 -0.4 Unregistered 0.02
2 Difenoconazole 0.01 100.0 0.006 -0.1 Unregistered 0.01
3 Fenvalerate 0.02 95.9 0.02 -0.6 Unregistered 0.04
4 Pyraclostrobin 0.03 88.7 0.003 -0.09 Unregistered 0.004
5 Thifluzamide 0.014 84.9 0.003 -0.2 Unregistered 0.02
6 Dimethomorph 0.2 69.8 0.001 -0.03 Unregistered 0.000 2
7 Diazinon 0.005 26.4 0.001 -0.002 Registered 0.000 6
8 Mandipropamid 0.2 18.9 0.001 Unregistered 0.000 0
9 Metalaxyl 0.08 8.3 0.1 -1.2 Registered 0.02
10 Propiconazole 0.07 7.5 0.03 -0.09 Registered 0.002
11 Fipronil - 3.8 0.01 Forbidden -
12 Phorate - 1.9 0.01 Forbidden -
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53批白术样品农药测定结果

, figureFileSmall=null, figureFileBig=null, tableContent=
No. Pesticide indicator ADI/mg·kg-1 bw Detection rate /% Residual amount/mg·kg-1 Registration status HQc [12]
1 Tebuconazole 0.03 100.0 0.06 -0.4 Unregistered 0.02
2 Difenoconazole 0.01 100.0 0.006 -0.1 Unregistered 0.01
3 Fenvalerate 0.02 95.9 0.02 -0.6 Unregistered 0.04
4 Pyraclostrobin 0.03 88.7 0.003 -0.09 Unregistered 0.004
5 Thifluzamide 0.014 84.9 0.003 -0.2 Unregistered 0.02
6 Dimethomorph 0.2 69.8 0.001 -0.03 Unregistered 0.000 2
7 Diazinon 0.005 26.4 0.001 -0.002 Registered 0.000 6
8 Mandipropamid 0.2 18.9 0.001 Unregistered 0.000 0
9 Metalaxyl 0.08 8.3 0.1 -1.2 Registered 0.02
10 Propiconazole 0.07 7.5 0.03 -0.09 Registered 0.002
11 Fipronil - 3.8 0.01 Forbidden -
12 Phorate - 1.9 0.01 Forbidden -
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白术中99种农药筛查分析及限量标准研究
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张万青 1 , 刘芫汐 2 , 金红宇 2 , 刘珍 1 , 王莹 2, * , 马双成 3 , 刘潇潇 1, *
中国药学杂志 | 论著 2025,60(6): 638-645
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中国药学杂志 | 论著 2025, 60(6): 638-645
白术中99种农药筛查分析及限量标准研究
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张万青1, 刘芫汐2, 金红宇2, 刘珍1, 王莹2, *, 马双成3, 刘潇潇1, *
作者信息
  • 1 广东省药品检验所, 广东省药品监督管理局中药质量控制与安全评价重点实验室, 广州 510663
  • 2 中国食品药品检定研究院, 北京 100050
  • 3 国家药典委员会, 北京 100061

    • 张万青,男,主管中药师 研究方向:中药农药残留检测与风险评估

通讯作者:

*王莹,女,博士,副研究员 研究方向:中药质量与安全 Tel:(010)53851413;
刘潇潇,女,博士,主任药师 研究方向:中药质量与安全 Tel:(020)32447998
Screening Analysis and Limit Standard Study of 99 Pesticides in Atractylodis Macrocephalae Rhizoma
Wanqing ZHANG1, Yuanxi LIU2, Hongyu JIN2, Zhen LIU1, Ying WANG2, *, Shuangcheng MA3, Xiaoxiao LIU1, *
Affiliations
  • 1 Key Laboratory of Traditional Chinese Medicine Quality Control and Safety Evaluation of Guangdong Provincial Drug Administration,Guangdong Institute for Drug Control, Guangzhou 510663, China
  • 2 National Institutes for Food and Drug Control, Beijing 100050, China
  • 3 Chinese Pharmacopoeia Commission, Beijing 100061, China
出版时间: 2025-03-22 doi: 10.11669/cpj.2025.06.010
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摘要
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目的 探索制定符合中药使用特点的白术中农药最大残留限量标准。方法 样品经QuEChERS法处理,采用气相色谱-串联质谱联用(GC-MS/MS)和液相色谱-串联质谱联用(LC-MS/MS)结合的方法对白术中99种农药指标进行筛查测定,同时对方法的灵敏度、回收率、重现性、精密度进行验证;采用符合中药特点的风险评估模式及转化原则,确定白术农药限量标准的指标及限度。结果 建立的白术中99种农药测定法符合方法学要求;53批白术样品中共检出农药12种,分别为:戊唑醇、苯醚甲环唑、氰戊菊酯和S-氰戊菊酯、吡唑醚菌酯、噻呋酰胺、烯酰吗啉、二嗪磷、双炔酰菌胺、精甲霜灵、丙环唑、氟虫腈、甲拌磷;按照GB2763转化指导原则将白术中二嗪磷限量标准转化为药品标准。结论 本研究有助于了解白术农药残留现状,可为其他中药品种农药残留限量标准的制定提供思路。

白术  /  GB 2763  /  农药残留  /  最大残留限量标准  /  二嗪磷

OBJECTIVE To explore the development of maximum residue limit standards for pesticides in Atractylodis Macrocephalae Rhizoma that conform to the characteristics of traditional Chinese medicine use. METHODS The samples were processed by QuEChERS method, and a combination of GC-MS/MS and LC-MS/MS was used to screen and determine 99 pesticide indicators in Atractylodis Macrocephalae Rhizoma. At the same time, the sensitivity, recovery rate, reproducibility, and precision of the method were verified. A risk assessment model and transformation principle that conforms to the characteristics of traditional Chinese medicine were adopted to determine the indicators and limits of the pesticide limit standards for Atractylodis Macrocephalae Rhizoma. RESULTS The established method for determining 99 pesticides in Atractylodis Macrocephalae Rhizoma meets the methodological requirements. A total of 12 pesticides were detected in 53 batches of Atractylodis Macrocephalae Rhizoma samples, including: tebuconazole, benzofenapyr, cypermethrin and S-cypermethrin, pyraclostrobin, thiamethoxam, enoxymorpholine, diazinon, propiconazole, fipronil, and methoxam. According to the GB2763 conversion guidelines, the limit standard for diazinon in Atractylodis Macrocephalae Rhizoma was converted into a drug standard. CONCLUSION This study helps to understand the risk of pesticide residues in Atractylodis Macrocephalae Rhizoma and provides ideas for the formulation of pesticide residue limit standards for traditional Chinese medicine.

Atractylodis Macrocephalae Rhizoma  /  GB 2763  /  pesticide residue  /  maximum residue limit standards  /  diazinon
张万青, 刘芫汐, 金红宇, 刘珍, 王莹, 马双成, 刘潇潇. 白术中99种农药筛查分析及限量标准研究. 中国药学杂志, 2025 , 60 (6) : 638 -645 . DOI: 10.11669/cpj.2025.06.010
Wanqing ZHANG, Yuanxi LIU, Hongyu JIN, Zhen LIU, Ying WANG, Shuangcheng MA, Xiaoxiao LIU. Screening Analysis and Limit Standard Study of 99 Pesticides in Atractylodis Macrocephalae Rhizoma[J]. Chinese Pharmaceutical Journal, 2025 , 60 (6) : 638 -645 . DOI: 10.11669/cpj.2025.06.010
正文
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白术为菊科植物白术(Atractylodes macrocephala Koidz.)的干燥根茎,能健脾益气、燥湿利水、止汗、安胎,用于脾虚食少、腹胀泄泻、痰饮眩悸、水肿、自汗、胎动不安[1]。白术为常见大宗中药,始载于《神农本草经》,在我国拥有悠久使用历史,既可作为中药材按药品管理,也可作为食品管理[2-3]。白术野生资源匮乏,市场上流通的主要为人工栽培生产,常见根腐病、白绢病、铁叶病、立枯病、白术长管蚜、小地老虎等病虫害[4]。白术种植中可选农药品种少、白术农药残留限量标准缺乏是白术农药管理的突出问题[5-7]。查询中国农药信息网农药登记数据中心,结果显示:截至2024年6月,已登记的白术农药主要为杀菌剂、杀虫剂、植物生长调节剂,如丙环唑、井冈霉素、二嗪磷、恶霉灵、精甲霜灵、嘧啶核苷类抗生素、氟啶胺、异菌脲、噻虫胺、高效氯氟氰菊酯、枯草芽孢杆菌、棉隆、氯化胆碱、噻虫胺等。农药残留标准控制方面,《GB 2763食品安全国家标准食品中农药最大残留限量》(以下简称GB 2763)中制定了白术中井冈霉素和二嗪磷的最大残留限量值(maximum residue limit,MRL)[8],《中国药典》2020年版四部通则“0212药材和饮片检定”下对植物类药材及饮片中的禁用农药33种,部分已登记农药在药材中并未建立质控标准。
本研究基于现行已登记使用的农药、GB 2763和《中国药典》2020年版农药指标,通过确定白术中检测的农药指标,建立农药指标的气相色谱-串联质谱联用(GC-MS/MS)和液相色谱-串联质谱联用(LC-MS/MS)检测方法,多批次样品筛查以及风险评估等步骤,初步拟定针对白术农药限量标准及配套检测方法。通过研究,为GB 2763标准与中药标准的转化提供思路,同时对白术上农药残留评估及登记研究工作,促进白术从种植到流通监管衔接有重要意义。
1 农药指标的确定
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1.1 白术登记农药
已登记产品涉及13种农药成分,其中嘧啶核苷类抗生素为含多种化合物,枯草芽孢杆菌属于豁免制定食品中最大残留限量标准的农药,氯化胆碱属于植物生长调节剂不列入检测指标。
1.2 常用农药指标的确定
GB 2763是食品中农药MRL的强制性国家标准,其中涉及药食同源的药用植物18种,依据课题组前期提出的“GB 2763中药品种限量标准转化原则”中涉及指标共40余种[9-10],其中白术的农药指标2个,根据农药理化性质,最终确定对44种农药进行筛查和监测。
1.3 禁用农药的确定
《中国药典》2020年版在通则0212中对植物类药材及饮片中的33种禁用农药作出了一致性限度规定,涉及农药成分55个。
2 材料与试药
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TQ 8040气相色谱串联三重串联四极杆质谱仪(日本岛津公司); WATERSXEVOTQS超高效液相色谱-串联三重串联四极杆质谱仪(美国WATERS公司); IKA KS 260 CTRL型振荡器、IKA MS 3 digital型涡旋器(德国IKA公司);ThermomySPIN 12型离心机(美国赛默飞公司);Millipore Q纯水系统。
55个禁用农药对照品溶液(中国食品药品检定研究院);35种农药混标溶液、7种杀虫剂和杀菌剂混标溶液、除虫菊素Ⅰ、除虫菊素Ⅱ、四聚乙醛、恶霉灵、异菌脲、噻虫胺、棉隆(天津阿尔塔科技有限公司);QuEChERS盐包(无水硫酸镁6 g、无水乙酸钠1.5 g)和QuEChERS净化包(无水硫酸镁900 mg、N-丙基乙二胺300 mg、十八烷基硅烷键合硅胶300 mg、硅胶300 mg、石墨化炭黑45 mg)(纳谱分析技术有限公司);甲醇、乙腈、甲酸为质谱级色谱纯;甲酸铵为质谱级;水为超纯水;冰乙酸为分析纯。
收集产地为安徽、河北、浙江、四川等,白术药材53批,所收样品均经广东省药品检验所主任药师刘潇潇鉴定为菊科植物白术(Atractylodes macrocephala Koidz.)的干燥根茎。
3 方法
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3.1 GC-MS/MS分析条件
弹性石英毛细管柱Agilent DB-5MS(0.25 mm×30 m,0.25 μm);进样口温度240 ℃,不分流进样,载气为高纯氦气(He),进样口为恒压模式,柱前压力为146 kPa。程序升温:初始温度70 ℃,保持2 min,先以25 ℃·min-1升温至150 ℃,再以3 ℃·min-1升温至200 ℃,最后以8 ℃·min-1升温至280 ℃,保持10 min。以三重四极杆串联质谱仪检测;离子源为电子轰击源(EI),离子源温度250 ℃。碰撞气为氮气。质谱传输接口温度280 ℃。质谱监测模式为多反应监测(MRM),各化合物参考保留时间(tR)、监测离子对、碰撞电压(CE)见表1。
3.2 LC-MS/MS分析条件
Aglient SB-C18色谱柱(3 mm×15 cm,2.7 μm);以体积分数0.05%甲酸溶液(含10 mmol·L-1甲酸铵)为流动相A,以体积分数0.05%甲酸的甲醇溶液(含10 mmol·L-1甲酸铵)为流动相B,梯度洗脱见表2;柱温为35 ℃,流速为0.4 mL·min-1。三重四极杆串联质谱仪检测;离子源为电喷雾(ESI)离子源,选择正离子/负离子切换扫描模式。监测模式为MRM,各化合物保留时间、监测离子对、CE参考值见表3。
3.3 溶液的制备
3.3.1 混合对照品溶液的制备
精密称取除虫菊素Ⅰ、除虫菊素Ⅱ、恶霉灵、异菌脲、噻虫胺和棉隆对照品适量,加乙腈制成4 μg·mL-1的储备溶液;精密量取55个禁用农药对照品溶液、35种农药混标溶液、7种杀虫剂和杀菌剂混标溶液、除虫菊素Ⅰ和除虫菊素Ⅱ适量,加乙腈分别制成1 μg·mL-1的溶液对照品溶液,密封,于-20 ℃冷藏保存。取不含待测指标的白术样品6 g,同供试品溶液制备方法处理成空白基质溶液。取空白基质溶液1 mL,氮吹浓缩至0.4 mL,精密加入对照品储备溶液5、10、20、50、100、200 μL后用乙腈稀释定容至1 mL,作为基质混合对照溶液。
3.3.2 供试品溶液的制备
取供试品,粉碎成粉末(过3号筛),取约3 g,精密称定,置50 mL聚苯乙烯具塞离心管中,加入体积分数1%冰乙酸溶液15 mL,涡旋使药粉充分浸润,放置30 min,精密加入乙腈15 mL,涡旋使混匀,置振荡器上剧烈振荡(每分钟500次)5 min,加入QuEChERS盐包,立即摇散,再置振荡器上剧烈振荡(每分钟500次)3 min,于冰浴中冷却10 min,离心(4 000 r·min-1)5 min,取上清液9 mL,置QuEChERS净化包,涡旋使充分混匀,再置振荡器上剧烈振荡(每分钟500次)5 min使净化完全,离心(4 000 r·min-1)5 min,分别精密吸取上清液1 mL,即得。
4 方法学考察
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4.1 线性方程及定量限检出限
各农药化合物在各自的线性范围内具有良好的线性,各农药相关系数均大于0.995,以线性最低点作为定量限,各化合物均能满足农药残留分析要求。
4.2 回收率及重复性试验
在空白样品中分别添加低、中、高(分别加入混合对照品工作液0.3、0.75、1.5 mL)3个水平的加标回收样品,每个水平3个平行实验,99个指标的加标回收率范围为62.9%~122.9%,相对标准偏差为0.7%~10.8%(表4)。
4.3 前处理方法的比较
不同前处理方式的农残结果存在一定差异,提取溶剂适量加水,甲拌磷、克百威、甲基异硫磷等农药残留的测试结果大都偏高[13],本实验样品白术均为干品,采用乙腈提取难以渗透到植物组织内部,为提高提取效率,选取QuEChers法提取。为克服基质影响,净化包材料包括无水硫酸镁、N-丙基乙二胺、十八烷基硅烷键合硅胶、硅胶300、石墨化炭黑。
5 农药检出情况汇总及风险评估
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5.1 检出农药情况
按照建立的分析方法,对53批白术药材进行农药残留量的测定,检出结果见表5。从表5结果看出,白术中禁用农药有2种检出,检出率较低,检出量均低于《中国药典》2020年版规定的定量限;除禁用农药外,其余检出10种农药,仅有3种为登记农药,戊唑醇、苯醚甲环唑、氰戊菊酯和S-氰戊菊酯、吡唑醚菌酯、噻呋酰胺等未登记农药成分检出率高于80%,说明白术种植过程中存在不当使用农药情况,白术农药登记工作有待完善;检出农药的慢性风险商(HQC)[9]均小于 1,认为其慢性摄入风险可接受。
5.2 检出农药的风险评估及标准转化
农药限度标准制定过程复杂耗时,专业性强,且成本高,《中国药典》2020年版规定可将我国食品安全国家标准相关残留限量转化为药品标准[11],基于此,本课题组前期提出“《GB 2763 食品安全国家标准 食品中农药最大残留限量》中药品种限量标准转化原则”。按照GB 2763-2021附录A分类,白术属于药用植物类,包括干品和鲜品,通过梳理白术农药残留限量标准共涉及2个农药指标,有MRL值4个,其中井冈霉素为水溶性农药,与其他农药混合易降解,需单独前处理,故暂不予以转化。按照拟定的农药转化原则,最终建议将GB 2763干品白术中农药残留限量标准转化为白术药品标准,二嗪磷MRLs值为0.1 mg·kg-1。二嗪磷采用GC-MS/MS和LC-MS/MS均可测试,对精密性、重复性、加样回收率、检测限等验证,两种检测手段均满足药典的要求。
6 结论
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本研究采用GC-MS/MS和LC-MS/MS法对白术中的99种农药进行检测,通过方法学验证表明建立的方法准确、灵敏,可应用于白术中农药测定。通过对53批白术样品进行分析发现,经慢性风险评估后认为此12种农药慢性摄入风险可接受。同时结合GB 2763白术(干)的残留限量标准及项目组前期拟定的农药转化原则,最终制定白术药材及饮片中农药最大残留限量值,即二嗪磷不得过0.1 mg·kg-1。
基金
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  • 国家药品监督管理局药品监管科学体系建设重点项目资助(RS2024Z006-110)
  • 2024年度国家药品标准制修订研究课题资助(2024Z01)
  • 广东省药品监督管理局科技创新项目资助(2024ZDZ14)
文献
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参考文献 引证文献
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2025年第60卷第6期
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doi: 10.11669/cpj.2025.06.010
  • 接收时间：2024-09-12
  • 首发时间：2025-11-07
  • 出版时间：2025-03-22
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出版历史
  • 收稿日期：2024-09-12
基金
国家药品监督管理局药品监管科学体系建设重点项目资助(RS2024Z006-110)
2024年度国家药品标准制修订研究课题资助(2024Z01)
广东省药品监督管理局科技创新项目资助(2024ZDZ14)
作者信息
    1 广东省药品检验所, 广东省药品监督管理局中药质量控制与安全评价重点实验室, 广州 510663
    2 中国食品药品检定研究院, 北京 100050
    3 国家药典委员会, 北京 100061

通讯作者:

*王莹,女,博士,副研究员 研究方向:中药质量与安全 Tel:(010)53851413;
刘潇潇,女,博士,主任药师 研究方向:中药质量与安全 Tel:(020)32447998
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https://castjournals.cast.org.cn/joweb/zgyxzz/CN/10.11669/cpj.2025.06.010
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2种不同金属材料的力学参数
科
Family		 属数
Number of
genus		 种数
Number of
species		 占总种数比例
Percentage of
total species (%)		 属
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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