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Article(id=1195816325735039912, tenantId=1146029695717560320, journalId=1190317699101192196, issueId=1195816324862624679, articleNumber=1001-2494(2024)24-2363-09, orderNo=null, doi=10.11669/cpj.2024.24.009, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1720972800000, receivedDateStr=2024-07-15, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1763034429248, onlineDateStr=2025-11-13, pubDate=1734796800000, pubDateStr=2024-12-22, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1763034429248, onlineIssueDateStr=2025-11-13, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1763034429248, creator=13701087609, updateTime=1763034429248, updator=13701087609, issue=Issue{id=1195816324862624679, tenantId=1146029695717560320, journalId=1190317699101192196, year='2024', volume='59', issue='24', pageStart='2299', pageEnd='2406', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=0, createTime=1763034429040, creator=13701087609, updateTime=1763034724390, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1195817563738390939, tenantId=1146029695717560320, journalId=1190317699101192196, issueId=1195816324862624679, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1195817563738390940, tenantId=1146029695717560320, journalId=1190317699101192196, issueId=1195816324862624679, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=2363, endPage=2371, ext={EN=ArticleExt(id=1195816326007669673, articleId=1195816325735039912, tenantId=1146029695717560320, journalId=1190317699101192196, language=EN, title=Research on the Revision of Maximum Residue Limits for Pesticides and the Establishment of Standard Residue Limits for Pesticides in Lilii Bulbus, columnId=null, journalTitle=Chinese Pharmaceutical Journal, columnName=null, runingTitle=null, highlight=null, articleAbstract=

OBJECTIVE To establish the limit standard of common pesticides in Lilii Bulbus, based on the “GB2763-2021 National Standard for Food Safety Maximum Residue Limit of Pesticides in food” and the multiple residue detection method of banned pesticides in Chinese medicinal materials and Chinese herbal decoction pieces (plants) in Chinese Pharmacopoeia. METHODS In accordance with the conversion tenet of the maximum residue limit(MRL) of pesticides in food established by the research group under the National Standard for Food Safety GB2763-2021, the converted types of agricultural residue limit of Lilii Bulbus were ascertained. The risk assessment of the MRL value was accomplished, and the detection methodologies for the agricultural residue of Lilii Bulbus were established to appraise the residue status of 50 batches of samples. RESULTS The QuEChERS procedure was adopted for extracting Lilii Bulbus, the gas chromatography-tandem mass spectrometry (GC-MS/MS) approach was utilized to determine six categories of pesticides, and the liquid chromatography-mass spectrometry (LC-MS/MS) method was implemented to determine nine sorts of pesticide residues. Meanwhile, the current prohibited pesticide multi-residue determination approach of the pharmacopoeia was taken into account. Comprehensive risk assessment and actual sample residue data were leveraged to establish the limits for ten kinds of pesticide residues in Lilii Bulbus. CONCLUSION The established method is precise and efficient and can be exploited for the determination of the residues of ten commonly utilized pesticides in Lilii Bulbus. The limited conversion principle of traditional Chinese medicine variety limit standard is applied to effectuate the conversion of ten pesticides of Lilii Bulbusin GB2763-2021, providing support for the safety assessment of Lilii Bulbus.

, correspAuthors=Jian SU, Shuangcheng MA, 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=Xiaolei WANG, Hao YUAN, Qi AN, Jian SU, Xueli LIU, Yongli LIU, Hongyu JIN, Shuangcheng MA), CN=ArticleExt(id=1195816400100049904, articleId=1195816325735039912, tenantId=1146029695717560320, journalId=1190317699101192196, language=CN, title=百合农药最大残留限量转化及百合农药残留限量标准研究, columnId=1190352405612040510, journalTitle=中国药学杂志, columnName=论著, runingTitle=null, highlight=null, articleAbstract=

目的 基于《GB2763-2021食品安全国家标准 食品中农药最大残留限量》与《中国药典》2020年版中药材及中药饮片(植物类)中禁用农药多残留检测法,制定百合中常用农药限量标准。方法 以课题组制定的《GB2763-2021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,确定百合农残限量转化品种,完成最大残留限量值的风险评估,建立百合农残气质联用、液质联用的检测方法,评价50批样品残留状况。结果 建立百合以QuEChERS法提取、气质法测定6种农药,液质法测定9种农药残留,同时兼顾现行《中国药典》禁用农药残留测定方法,综合风险评估及实际样品残留数据,确定百合中10种农药残留限量。。结论 研究建立的方法可用于百合中10种常用农药残留测定,准确、高效。应用中药品种限量标准转化原则完成GB2763-2021百合(干)中的10种农药限度转化,为百合安全性评价提供支撑。

, correspAuthors=苏建, 马双成, authorNote=null, correspAuthorsNote=
* 苏建,男,硕士,正高级工程师 研究方向:中药质量及中药安全研究 Tel:(010)53852484;
马双成,男,博士,研究员 研究方向:中药质量与安全研究 Tel:(0311)69086155
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王晓蕾与袁浩为共同第一作者

王晓蕾,女,硕士,副主任药师 研究方向:中药质量与安全研究;

袁浩,男,高级工程师 研究方向:中药质量与安全研究。

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王晓蕾,女,硕士,副主任药师 研究方向:中药质量与安全研究;

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王晓蕾,女,硕士,副主任药师 研究方向:中药质量与安全研究;

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袁浩,男,高级工程师 研究方向:中药质量与安全研究。

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袁浩,男,高级工程师 研究方向:中药质量与安全研究。

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Digital Chin Med(数字中医药), 2023, 6 (4): 426-437., articleTitle=Identification of metabolites in different parts of JuandanBaihe (Liliumlancifolium) by UPLC-Q-TOF-MS and their hypoglycemic activities, refAbstract=null), Reference(id=1196081614640951487, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816325735039912, doi=null, pmid=null, pmcid=null, year=2020, volume=null, issue=null, pageStart=276, pageEnd=null, url=null, language=null, rfNumber=[16], rfOrder=15, authorNames=null, journalName=Ch.P(2020)Vol Ⅴ(中国药典2020年版四部), refType=null, unstructuredReference=Ch.P(2020)Vol Ⅴ(中国药典2020年版四部)[S]. 2020: 276., articleTitle=null, refAbstract=null), Reference(id=1196081614720643264, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816325735039912, doi=null, pmid=null, pmcid=null, year=2020, volume=40, issue=10, pageStart=1877, pageEnd=1881, url=null, language=null, rfNumber=[17], rfOrder=16, authorNames=WANG X L, LIU Y L, SU J, journalName=Chin J Pharm Anal(药物分析杂志), refType=null, unstructuredReference=WANG X L, LIU Y L, SU J, et al. Guideline for quality control in analysis of harmful residues in traditional Chinese medicines[J]. Chin J Pharm Anal(药物分析杂志), 2020, 40(10):1877-1881., articleTitle=Guideline for quality control in analysis of harmful residues in traditional Chinese medicines, refAbstract=null)], funds=[Fund(id=1196081612157923500, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816325735039912, awardId=2023SKLDRS0103, language=CN, fundingSource=药品监管科学全国重点实验室第一批课题(2023SKLDRS0103), fundOrder=null, country=null), Fund(id=1196081612216643757, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816325735039912, 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(RS2024Z006-110), fundOrder=null, country=null), Fund(id=1196081612304724142, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816325735039912, awardId=2024Z01, language=CN, fundingSource=2024年度国家药品标准制修订研究课题(2024Z01), fundOrder=null, country=null), Fund(id=1196081612384415919, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816325735039912, awardId=null, language=CN, fundingSource=河北省中医药管理局科研计划重点项目, fundOrder=null, country=null)], companyList=[AuthorCompany(id=1196081606394949723, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816325735039912, xref=1, ext=[AuthorCompanyExt(id=1196081606411726940, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816325735039912, companyId=1196081606394949723, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1 NMPA Key Laboratory for Quality Monitoring and Evaluation of Traditional Chinese Medicine (Chinese Materia Medica), Hebei Institute for Drug and Medical Device Control, Shijiazhuang 050227, China), AuthorCompanyExt(id=1196081606420115549, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816325735039912, companyId=1196081606394949723, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1 河北省药品医疗器械检验研究院, 国家药品监督管理局中药材质量监测评价重点实验室, 石家庄 050227)]), AuthorCompany(id=1196081606504001630, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816325735039912, xref=2, ext=[AuthorCompanyExt(id=1196081606512390239, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816325735039912, companyId=1196081606504001630, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=2 National Institutes for Food and Drug Control, Beijing 102629, China), AuthorCompanyExt(id=1196081606520778848, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816325735039912, companyId=1196081606504001630, 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 102629)]), AuthorCompany(id=1196081606613053538, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816325735039912, xref=3, ext=[AuthorCompanyExt(id=1196081606625636451, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816325735039912, companyId=1196081606613053538, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=3 Chinese Pharmacopoeia Commission, Beijing 100061, China), AuthorCompanyExt(id=1196081606638219364, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816325735039912, companyId=1196081606613053538, 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=1196081610580865176, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816325735039912, language=EN, label=Fig.1, caption=EIC of LLOQ in Lilii Bulbus, figureFileSmall=CxCQTONOy0b4LM6IG/2kxw==, figureFileBig=WxlAuimMYPsQHd5iT1jx5Q==, tableContent=null), ArticleFig(id=1196081610660556953, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816325735039912, language=CN, label=图1, caption=百合中各农药定量下限提取离子流图, figureFileSmall=CxCQTONOy0b4LM6IG/2kxw==, figureFileBig=WxlAuimMYPsQHd5iT1jx5Q==, tableContent=null), ArticleFig(id=1196081610744443034, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816325735039912, language=EN, label=Fig.2, caption=TIC of GC-MS/MS(1) and LC-MS/MS(2) of samples and reference solutions

A-negative sample; B-positive sample; C-reference substance in negative sample.

, figureFileSmall=68dQ6frVyMQXXwwgjr9+Ng==, figureFileBig=b9Nq5dMLMntXxt0Djwjwew==, tableContent=null), ArticleFig(id=1196081610798968987, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816325735039912, language=CN, label=图2, caption=百合样品、对照品溶液的GC-MS/MS(1)与LC-MS/MS(2)典型总离子流图(TIC)

A-空白基质; B-阳性样品; C-基质混合对照品。

, figureFileSmall=68dQ6frVyMQXXwwgjr9+Ng==, figureFileBig=b9Nq5dMLMntXxt0Djwjwew==, tableContent=null), ArticleFig(id=1196081610857689244, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816325735039912, language=EN, label=Tab.1, caption=

Pesticide limit information for Lilii Bulbus in GB2763-2021

, figureFileSmall=null, figureFileBig=null, tableContent=
Serial number Pesticide name Types MRL of Lilii Bulbus(dry)/mg·kg-1 MRL of Lilii Bulbus(fresh)/mg·kg-1
1 Chlorothalonil Bactericide 0.05 0.05
2 Acetamiprid Insecticide 0.05 0.05
3 Difenoconazole Bactericide 0.05 0.05
4 Pyraclostrobin Bactericide 0.1 0.05
5 Propiconazole Bactericide 0.05 0.05
6 Cyprodinil Bactericide 1 0.5
7 Tebufenozide Insecticide 0.1 0.05
8 Pymetrozin Insecticide 0.05 0.05
9 Epoxiconazole Bactericide 0.2 0.1
10 Abamectin Bactericide 0.05 0.05
11 Glyphosate Herbicide No limit 0.2
12 Zineb Bactericide 2 0.5
), ArticleFig(id=1196081610920603805, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816325735039912, language=CN, label=表1, caption=

GB2763-2021中百合农药最大残留限量(MRL)信息

, figureFileSmall=null, figureFileBig=null, tableContent=
Serial number Pesticide name Types MRL of Lilii Bulbus(dry)/mg·kg-1 MRL of Lilii Bulbus(fresh)/mg·kg-1
1 Chlorothalonil Bactericide 0.05 0.05
2 Acetamiprid Insecticide 0.05 0.05
3 Difenoconazole Bactericide 0.05 0.05
4 Pyraclostrobin Bactericide 0.1 0.05
5 Propiconazole Bactericide 0.05 0.05
6 Cyprodinil Bactericide 1 0.5
7 Tebufenozide Insecticide 0.1 0.05
8 Pymetrozin Insecticide 0.05 0.05
9 Epoxiconazole Bactericide 0.2 0.1
10 Abamectin Bactericide 0.05 0.05
11 Glyphosate Herbicide No limit 0.2
12 Zineb Bactericide 2 0.5
), ArticleFig(id=1196081611000295582, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816325735039912, language=EN, label=Tab.2, caption=

Results of risk quotient in Lilii Bulbus

, figureFileSmall=null, figureFileBig=null, tableContent=
Serial No. Pesticide name MRL/mg·kg-1 ADI/mg·kg-1bw ARfD/mg·kg-1bw HQc HQa
1 Chlorothalonil 0.05 0.02 0.6 0.003 ≤1
2 Acetamiprid 0.05 0.07 0.1 0.001
3 Difenoconazole 0.05 0.01 0.3 0.005
4 Pyraclostrobin 0.1 0.03 0.05 0.004
5 Propiconazole 0.05 0.07 0.3 0.001
6 Cyprodinil 1 0.03 / 0.035
7 Tebufenozide 0.1 0.02 0.9 0.005
8 Pymetrozin 0.05 0.03 0.1 0.002
9 Epoxiconazole 0.2 0.02 0.023 0.011
10 Abamectin 0.05 0.001 / 0.053
11 Zineb 2 0.03 / 0.070
), ArticleFig(id=1196081611067404447, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816325735039912, language=CN, label=表2, caption=

百合中农药限量风险商结果

, figureFileSmall=null, figureFileBig=null, tableContent=
Serial No. Pesticide name MRL/mg·kg-1 ADI/mg·kg-1bw ARfD/mg·kg-1bw HQc HQa
1 Chlorothalonil 0.05 0.02 0.6 0.003 ≤1
2 Acetamiprid 0.05 0.07 0.1 0.001
3 Difenoconazole 0.05 0.01 0.3 0.005
4 Pyraclostrobin 0.1 0.03 0.05 0.004
5 Propiconazole 0.05 0.07 0.3 0.001
6 Cyprodinil 1 0.03 / 0.035
7 Tebufenozide 0.1 0.02 0.9 0.005
8 Pymetrozin 0.05 0.03 0.1 0.002
9 Epoxiconazole 0.2 0.02 0.023 0.011
10 Abamectin 0.05 0.001 / 0.053
11 Zineb 2 0.03 / 0.070
), ArticleFig(id=1196081611138707616, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816325735039912, language=EN, label=Tab.3, caption=

Pesticides and related chemicals, retention time of internal standard compounds, monitoring ion pairs and collision voltage (CE) in Lilli Bulbus by LC-MS/MS

, figureFileSmall=null, figureFileBig=null, tableContent=
Serial No. Pesticide name tR/min Mode m/z (Mother ion) m/z (Daughter ion) CE /V
1 Pymetrozin 0.95 + 218.2 105.2 -22
218.2 78.1 -41
2 Tebufenozide 9.31 + 353.2 133.1 -20
353.2 297.1 -8
3 Pyraclostrobin 9.95 + 388.1 296.1 -19
388.1 194.1 -17
4 Acetamiprid 2.74 + 223.1 126.0 -22
223.1 56.1 -15
5 Difenoconazole 10.28 + 406.1 337.0 -17
406.1 251.0 -25
6 Propiconazole 9.73 + 342.0 159.1 -30
342.0 205.1 -18
7 Epoxiconazole 8.95 + 330.1 121.2 -21
330.1 141.1 -18
8 Cyprodinil 9.16 + 226.1 93.1 -34
226.1 108.1 -27
9 Abamectin 12.53 + 895.6 449.3 -50
895.6 751.3 -45
10 Chlorothalonil 5.79 - 244.9 181.9 35
244.9 174.9 32
), ArticleFig(id=1196081611230982305, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816325735039912, language=CN, label=表3, caption=

LC-MS/MS法测定百合中各农药及相关化学品、内标化合物保留时间、监测离子对及碰撞电压(CE)参考值

, figureFileSmall=null, figureFileBig=null, tableContent=
Serial No. Pesticide name tR/min Mode m/z (Mother ion) m/z (Daughter ion) CE /V
1 Pymetrozin 0.95 + 218.2 105.2 -22
218.2 78.1 -41
2 Tebufenozide 9.31 + 353.2 133.1 -20
353.2 297.1 -8
3 Pyraclostrobin 9.95 + 388.1 296.1 -19
388.1 194.1 -17
4 Acetamiprid 2.74 + 223.1 126.0 -22
223.1 56.1 -15
5 Difenoconazole 10.28 + 406.1 337.0 -17
406.1 251.0 -25
6 Propiconazole 9.73 + 342.0 159.1 -30
342.0 205.1 -18
7 Epoxiconazole 8.95 + 330.1 121.2 -21
330.1 141.1 -18
8 Cyprodinil 9.16 + 226.1 93.1 -34
226.1 108.1 -27
9 Abamectin 12.53 + 895.6 449.3 -50
895.6 751.3 -45
10 Chlorothalonil 5.79 - 244.9 181.9 35
244.9 174.9 32
), ArticleFig(id=1196081611306479778, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816325735039912, language=EN, label=Tab.4, caption=

Pesticides and related chemicals, retention time of internal standard(IS) compounds, monitoring ion pairs and collision voltage (CE) in Lilli Bulbus by GC-MS/MS

, figureFileSmall=null, figureFileBig=null, tableContent=
Serial No. Pesticides tR/min m/z(Mother ion) m/z(Daughter ion) CE /V
1 Chlorothalonil 17.83 263.9 168.0 24
263.9 228.8 14
265.9 168.0 22
2 Difenoconazole 45.23 323.0 265.0 14
265.0 202.0 20
265.0 139.0 30
3 Acetamiprid 40.10 152.0 116.0 18
152.0 89.0 26
221.0 56.0 22
4 Propiconazole 35.00/35.26 173.0 109.0 28
173.0 145.0 16
259.0 69.0 14
5 Cyprodinil 23.58 225.2 224.3 16
224.1 208.1 22
224.1 197.1 14
6 Epoxiconazole 37.38 192.0 138.0 14
192.0 111.1 24
192.0 102.1 26
7 Triphenyl phosphate(IS) 37.08 326.0 233.0 12
326.0 215.0 21
326.0 169.0 30
), ArticleFig(id=1196081611407143075, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816325735039912, language=CN, label=表4, caption=

GC-MS/MS测定百合中各农药及相关化学品、内标化合物保留时间、监测离子对及碰撞电压(CE)参考值

, figureFileSmall=null, figureFileBig=null, tableContent=
Serial No. Pesticides tR/min m/z(Mother ion) m/z(Daughter ion) CE /V
1 Chlorothalonil 17.83 263.9 168.0 24
263.9 228.8 14
265.9 168.0 22
2 Difenoconazole 45.23 323.0 265.0 14
265.0 202.0 20
265.0 139.0 30
3 Acetamiprid 40.10 152.0 116.0 18
152.0 89.0 26
221.0 56.0 22
4 Propiconazole 35.00/35.26 173.0 109.0 28
173.0 145.0 16
259.0 69.0 14
5 Cyprodinil 23.58 225.2 224.3 16
224.1 208.1 22
224.1 197.1 14
6 Epoxiconazole 37.38 192.0 138.0 14
192.0 111.1 24
192.0 102.1 26
7 Triphenyl phosphate(IS) 37.08 326.0 233.0 12
326.0 215.0 21
326.0 169.0 30
), ArticleFig(id=1196081611474251940, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816325735039912, language=EN, label=Tab.5, caption=

Standard curve information of 10 pesticides in lilli Bulbus

, figureFileSmall=null, figureFileBig=null, tableContent=
Method Serial No. Pesticides Linear range /ng·mL-1 Linear equation r
GC-MS/MS 1 Chlorothalonil 2.5 -250 Y=1.096e-2X-4.580e-2 0.998
2 Difenoconazole 1 -50 Y=0.354 0X+5.997 1e-2 0.998
3 Acetamiprid 2 -100 Y=2.935 9e-2X+3.915 7e-2 0.999
4 Propiconazole 0.5 -25 Y=0.129 1X+2.402 0 0.999
5 Cyprodinil 1 -100 Y=0.114 2X+0.110 9 0.999
6 Epoxiconazole 0.5 -50 Y=0.117 6X+5.401 6 0.999
LC-MS/MS 1 Pymetrozin 1 -100 Y=67 851.6X+4 670.8 0.995
2 Difenoconazole 0.5 -50 Y=53 981.8X+360.4 0.998
3 Tebufenozide 0.25 -25 Y=39 012.9X-581.4 0.998
4 Propiconazole 0.25 -25 Y=18 630.7X-1 848.0 0.998
5 Pyraclostrobin 0.25 -25 Y=25 088.1X+1 551.5 0.997
6 Epoxiconazole 0.5 -50 Y=40 995.2X+2 986.2 0.998
7 Acetamiprid 1 -100 Y=64 184.4X+1 997.7 0.998
8 Cyprodinil 1 -100 Y=26 086.9X+3 516.3 0.996
9 Abamectin 0.25 -25 Y=72.1X-25.2 0.990
10 Chlorothalonil 2.5 -250 Y=246.3X+12.5 0.990
), ArticleFig(id=1196081611541360805, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816325735039912, language=CN, label=表5, caption=

百合中10种农药的标准曲线信息

, figureFileSmall=null, figureFileBig=null, tableContent=
Method Serial No. Pesticides Linear range /ng·mL-1 Linear equation r
GC-MS/MS 1 Chlorothalonil 2.5 -250 Y=1.096e-2X-4.580e-2 0.998
2 Difenoconazole 1 -50 Y=0.354 0X+5.997 1e-2 0.998
3 Acetamiprid 2 -100 Y=2.935 9e-2X+3.915 7e-2 0.999
4 Propiconazole 0.5 -25 Y=0.129 1X+2.402 0 0.999
5 Cyprodinil 1 -100 Y=0.114 2X+0.110 9 0.999
6 Epoxiconazole 0.5 -50 Y=0.117 6X+5.401 6 0.999
LC-MS/MS 1 Pymetrozin 1 -100 Y=67 851.6X+4 670.8 0.995
2 Difenoconazole 0.5 -50 Y=53 981.8X+360.4 0.998
3 Tebufenozide 0.25 -25 Y=39 012.9X-581.4 0.998
4 Propiconazole 0.25 -25 Y=18 630.7X-1 848.0 0.998
5 Pyraclostrobin 0.25 -25 Y=25 088.1X+1 551.5 0.997
6 Epoxiconazole 0.5 -50 Y=40 995.2X+2 986.2 0.998
7 Acetamiprid 1 -100 Y=64 184.4X+1 997.7 0.998
8 Cyprodinil 1 -100 Y=26 086.9X+3 516.3 0.996
9 Abamectin 0.25 -25 Y=72.1X-25.2 0.990
10 Chlorothalonil 2.5 -250 Y=246.3X+12.5 0.990
), ArticleFig(id=1196081611604275366, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816325735039912, language=EN, label=Tab.6, caption=

Data of precision, recovery and sensitivity of 10 pesticides in lilli Bulbus

, figureFileSmall=null, figureFileBig=null, tableContent=
Method Serial
No.		 Pesticides Recovery/% Average
recovery/%		 Precision
/%		 Lower limit of quantitation
(LLOQ)/mg·kg-1
Low Median High
GC-MS/MS 1 Chlorothalonil 77.87 115.01 100.28 100.3 5.8 0.002 5
2 Difenoconazole 76.65 108.59 96.72 99.1 9.1 0.01
3 Acetamiprid 81.05 104.42 96.72 91.2 6.2 0.02
4 Propiconazole 86.32 95.04 97.06 96.7 4.8 0.005
5 Cyprodinil 77.97 88.54 91.21 96.7 3.1 0.01
6 Epoxiconazole 88.46 102.53 99.17 97.1 10.8 0.005
LC-MS/MS 1 Pymetrozin 102.82 88.90 92.96 93.0 0.4 0.01
2 Difenoconazole 103.00 86.57 91.30 97.7 1.1 0.005
3 Tebufenozide 105.54 93.07 96.33 97.4 2.6 0.002 5
4 Propiconazole 113.56 90.00 97.35 97.7 2.8 0.002 5
5 Pyraclostrobin 102.86 94.97 97.68 92.1 2.2 0.002 5
6 Epoxiconazole 104.17 91.97 92.09 104.9 1.7 0.005
7 Acetamiprid 112.97 101.85 104.87 91.3 0.9 0.01
8 Cyprodinil 102.58 97.56 97.69 96.3 1.0 0.01
9 Abamectin 92.64 87.50 84.98 85.0 8.1 0.0025
), ArticleFig(id=1196081611688161447, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816325735039912, language=CN, label=表6, caption=

百合中10种农药的精密度、回收率及灵敏度数据

, figureFileSmall=null, figureFileBig=null, tableContent=
Method Serial
No.		 Pesticides Recovery/% Average
recovery/%		 Precision
/%		 Lower limit of quantitation
(LLOQ)/mg·kg-1
Low Median High
GC-MS/MS 1 Chlorothalonil 77.87 115.01 100.28 100.3 5.8 0.002 5
2 Difenoconazole 76.65 108.59 96.72 99.1 9.1 0.01
3 Acetamiprid 81.05 104.42 96.72 91.2 6.2 0.02
4 Propiconazole 86.32 95.04 97.06 96.7 4.8 0.005
5 Cyprodinil 77.97 88.54 91.21 96.7 3.1 0.01
6 Epoxiconazole 88.46 102.53 99.17 97.1 10.8 0.005
LC-MS/MS 1 Pymetrozin 102.82 88.90 92.96 93.0 0.4 0.01
2 Difenoconazole 103.00 86.57 91.30 97.7 1.1 0.005
3 Tebufenozide 105.54 93.07 96.33 97.4 2.6 0.002 5
4 Propiconazole 113.56 90.00 97.35 97.7 2.8 0.002 5
5 Pyraclostrobin 102.86 94.97 97.68 92.1 2.2 0.002 5
6 Epoxiconazole 104.17 91.97 92.09 104.9 1.7 0.005
7 Acetamiprid 112.97 101.85 104.87 91.3 0.9 0.01
8 Cyprodinil 102.58 97.56 97.69 96.3 1.0 0.01
9 Abamectin 92.64 87.50 84.98 85.0 8.1 0.0025
), ArticleFig(id=1196081611755270312, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1195816325735039912, language=EN, label=Tab.7, caption=

Results of pesticide residues in Lilii Bulbus samples

, figureFileSmall=null, figureFileBig=null, tableContent=
Serial number Pesticide name MRL/mg·kg-1 Range of results/mg·kg-1 Detection rate /% Over standard rate /%
1 Chlorothalonil 0.05 - 0 0
2 Acetamiprid 0.05 0.01-0.03 16 0
3 Difenoconazole 0.05 0.007-0.126 38 4
4 Pyraclostrobin 0.1 0.004-0.257 50 16
5 Propiconazole 0.05 0.003-0.049 8 0
6 Cyprodinil 1 - 0 0
7 Tebufenozide 0.1 0.003-0.28 22 0
8 Pymetrozin 0.05 - 0 0
9 Epoxiconazole 0.2 0.008-0.020 4 0
10 Abamectin 0.05 - 0 0
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百合样品农药残留量结果

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Serial number Pesticide name MRL/mg·kg-1 Range of results/mg·kg-1 Detection rate /% Over standard rate /%
1 Chlorothalonil 0.05 - 0 0
2 Acetamiprid 0.05 0.01-0.03 16 0
3 Difenoconazole 0.05 0.007-0.126 38 4
4 Pyraclostrobin 0.1 0.004-0.257 50 16
5 Propiconazole 0.05 0.003-0.049 8 0
6 Cyprodinil 1 - 0 0
7 Tebufenozide 0.1 0.003-0.28 22 0
8 Pymetrozin 0.05 - 0 0
9 Epoxiconazole 0.2 0.008-0.020 4 0
10 Abamectin 0.05 - 0 0
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Comparison of recoveries of LIlli Bulbus sample solution by different preparation methods

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Serial
number		 Pesticide
name		 The recovery rate-soaked
by water/%		 The recovery rate-soaked
by water added acid /%
1 Chlorothalonil 61.2 96.9
2 Acetamiprid 69.7 85.9
3 Difenoconazole 83.9 85.2
4 Pyraclostrobin 93.4 92.5
5 Propiconazole 86.2 87.0
6 Cyprodinil 77.5 86.5
7 Tebufenozide 98.5 89.1
8 Pymetrozin 92.6 80.8
9 Epoxiconazole 92.7 95.6
10 Abamectin 85.8 90.3
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百合供试品溶液制备方法考察回收率对比

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Serial
number		 Pesticide
name		 The recovery rate-soaked
by water/%		 The recovery rate-soaked
by water added acid /%
1 Chlorothalonil 61.2 96.9
2 Acetamiprid 69.7 85.9
3 Difenoconazole 83.9 85.2
4 Pyraclostrobin 93.4 92.5
5 Propiconazole 86.2 87.0
6 Cyprodinil 77.5 86.5
7 Tebufenozide 98.5 89.1
8 Pymetrozin 92.6 80.8
9 Epoxiconazole 92.7 95.6
10 Abamectin 85.8 90.3
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百合农药最大残留限量转化及百合农药残留限量标准研究
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王晓蕾 1 , 袁浩 1 , 安琪 1 , 苏建 1, * , 刘雪莉 1 , 刘永利 1 , 金红宇 2 , 马双成 3, *
中国药学杂志 | 论著 2024,59(24): 2363-2371
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中国药学杂志 | 论著 2024, 59(24): 2363-2371
百合农药最大残留限量转化及百合农药残留限量标准研究
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王晓蕾1, 袁浩1, 安琪1, 苏建1, *, 刘雪莉1, 刘永利1, 金红宇2, 马双成3, *
作者信息
  • 1 河北省药品医疗器械检验研究院, 国家药品监督管理局中药材质量监测评价重点实验室, 石家庄 050227
  • 2 中国食品药品检定研究院, 北京 102629
  • 3 国家药典委员会, 北京 100061

    • 王晓蕾,女,硕士,副主任药师 研究方向:中药质量与安全研究;

    袁浩,男,高级工程师 研究方向:中药质量与安全研究。

通讯作者:

* 苏建,男,硕士,正高级工程师 研究方向:中药质量及中药安全研究 Tel:(010)53852484;
马双成,男,博士,研究员 研究方向:中药质量与安全研究 Tel:(0311)69086155
Research on the Revision of Maximum Residue Limits for Pesticides and the Establishment of Standard Residue Limits for Pesticides in Lilii Bulbus
Xiaolei WANG1, Hao YUAN1, Qi AN1, Jian SU1, *, Xueli LIU1, Yongli LIU1, Hongyu JIN2, Shuangcheng MA3, *
Affiliations
  • 1 NMPA Key Laboratory for Quality Monitoring and Evaluation of Traditional Chinese Medicine (Chinese Materia Medica), Hebei Institute for Drug and Medical Device Control, Shijiazhuang 050227, China
  • 2 National Institutes for Food and Drug Control, Beijing 102629, China
  • 3 Chinese Pharmacopoeia Commission, Beijing 100061, China
出版时间: 2024-12-22 doi: 10.11669/cpj.2024.24.009
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摘要
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目的 基于《GB2763-2021食品安全国家标准 食品中农药最大残留限量》与《中国药典》2020年版中药材及中药饮片(植物类)中禁用农药多残留检测法,制定百合中常用农药限量标准。方法 以课题组制定的《GB2763-2021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,确定百合农残限量转化品种,完成最大残留限量值的风险评估,建立百合农残气质联用、液质联用的检测方法,评价50批样品残留状况。结果 建立百合以QuEChERS法提取、气质法测定6种农药,液质法测定9种农药残留,同时兼顾现行《中国药典》禁用农药残留测定方法,综合风险评估及实际样品残留数据,确定百合中10种农药残留限量。。结论 研究建立的方法可用于百合中10种常用农药残留测定,准确、高效。应用中药品种限量标准转化原则完成GB2763-2021百合(干)中的10种农药限度转化,为百合安全性评价提供支撑。

百合  /  农药  /  《GB2763-2021食品安全国家标准 食品中农药最大残留限量》  /  标准转化  /  残留限量

OBJECTIVE To establish the limit standard of common pesticides in Lilii Bulbus, based on the “GB2763-2021 National Standard for Food Safety Maximum Residue Limit of Pesticides in food” and the multiple residue detection method of banned pesticides in Chinese medicinal materials and Chinese herbal decoction pieces (plants) in Chinese Pharmacopoeia. METHODS In accordance with the conversion tenet of the maximum residue limit(MRL) of pesticides in food established by the research group under the National Standard for Food Safety GB2763-2021, the converted types of agricultural residue limit of Lilii Bulbus were ascertained. The risk assessment of the MRL value was accomplished, and the detection methodologies for the agricultural residue of Lilii Bulbus were established to appraise the residue status of 50 batches of samples. RESULTS The QuEChERS procedure was adopted for extracting Lilii Bulbus, the gas chromatography-tandem mass spectrometry (GC-MS/MS) approach was utilized to determine six categories of pesticides, and the liquid chromatography-mass spectrometry (LC-MS/MS) method was implemented to determine nine sorts of pesticide residues. Meanwhile, the current prohibited pesticide multi-residue determination approach of the pharmacopoeia was taken into account. Comprehensive risk assessment and actual sample residue data were leveraged to establish the limits for ten kinds of pesticide residues in Lilii Bulbus. CONCLUSION The established method is precise and efficient and can be exploited for the determination of the residues of ten commonly utilized pesticides in Lilii Bulbus. The limited conversion principle of traditional Chinese medicine variety limit standard is applied to effectuate the conversion of ten pesticides of Lilii Bulbusin GB2763-2021, providing support for the safety assessment of Lilii Bulbus.

Lilii Bulbus  /  pesticide  /  GB2763-2021  /  standard conversion  /  residue limit
王晓蕾, 袁浩, 安琪, 苏建, 刘雪莉, 刘永利, 金红宇, 马双成. 百合农药最大残留限量转化及百合农药残留限量标准研究. 中国药学杂志, 2024 , 59 (24) : 2363 -2371 . DOI: 10.11669/cpj.2024.24.009
Xiaolei WANG, Hao YUAN, Qi AN, Jian SU, Xueli LIU, Yongli LIU, Hongyu JIN, Shuangcheng MA. Research on the Revision of Maximum Residue Limits for Pesticides and the Establishment of Standard Residue Limits for Pesticides in Lilii Bulbus[J]. Chinese Pharmaceutical Journal, 2024 , 59 (24) : 2363 -2371 . DOI: 10.11669/cpj.2024.24.009
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百合为历史悠久的药食两用品种,始载于《神农本草经》,列为中品。性甘、寒;归心、肺经;用于养阴润肺,清心安神[1]。百合属植物约有115种[2],《本草纲目》记载百合分为白花类百合、红花类山丹、红黄花类卷丹3类,均可食用,仅白花类百合药用。《中国药典》2020年版收载百合为百合科植物卷丹(Lilium lancifolium Thunb.)、百合(Lilium brownii F. E. Brown var. viridulum Baker) 或细叶百合(Lilium pumilum DC.)的干燥肉质鳞叶。秋季采挖,洗净,剥取鳞叶,置沸水中略烫,干燥,炮制品为蜜百合。其中卷丹为药用百合的主流品种,主要栽培于湖南、湖北、安徽、江西等地[3-4]。兰州百合(Lilimdar)为甘肃省地方习用品,主产于甘肃兰州、临洮等地[5]。
百合种植易感染病虫害,特别是枯萎病、灰霉病、炭疽病、线虫病等[6],不仅严重影响产量,还影响性状、成分含量及构成[7],经查询农业部百合登记农药数量较少,故实际种植中存在过量及频繁叠加品种使用的情况[8],易造成安全隐患。Peng等[9]在百合中检出了敌敌畏、乐果、甲基异柳磷、毒死蜱4种有机磷农药,《中国药典》2020年版四部增订中药材与中药饮片(植物类)中33种禁用农药多残留测定法及不得检出的规定后,未见百合中禁用农药检出的报道,出现氯虫苯甲酰胺、代森锌、腐霉利等农残的检出[10-11]。可见市场和监管的需求是动态变化的,顺应发展持续完善中药材及中药饮片农药残留限量标准是十分必要的。
农业部发布的《GB2763-2021食品安全国家标准 食品中农药最大残留限量》是我国食品中农药最大残留限量的强制性国家标准,基本全面覆盖了农产品的农药使用品种[12],于2021年版始收录药食同源物质百合的限量标准。本研究按照课题组前期提出的《GB2763-2021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[13],拟转化百合项下农药最大残留限量(MRL),通过以百合常用农药MRL进行风险评估,确定测定指标,考察农药品种的检测参数,参照《中国药典》2020年版禁用农药多残留测定法的色谱质谱条件,测定50批百合样品作为验证,完成制定百合中常用农药残留限量标准,为百合农药残留安全性风险管控提供技术支撑,同时也为探索GB2763-2021转化为中药标准的模式贡献数据。
1 试验材料
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1.1 仪器
LCMS-8050型高效液相色谱-三重四极杆质谱联用仪、GCMS-TQ8050NX型气相色谱-三重四极杆质谱联用仪(日本岛津公司);AE240型电子分析天平(瑞士METTLER TOLEDO公司);精密移液器(德国eppendorf公司);色谱柱:Shim-pack Velox C18(2.1 mm×100 mm,1.8 μm)、SH-Rxi-17sil毛细管柱(0.25 mm× 30 m, 0.25 μm)(日本岛津公司)。
1.2 试剂与试药
乙腈、甲醇(色谱纯),甲酸、甲酸铵为色谱纯,水为蒸馏水(广州屈臣氏食品饮料有限公司)。
1.3 对照品
方法建立使用对照品溶液购自天津阿尔塔科技有限公司单标、10种农药混标(批号:SGLC23-3900-31)购自岛津公司,各农药质量浓度均为100 μg·mL-1;方法验证使用10种农药混标购自天津阿尔塔科技有限公司(批号:S173279),百菌清、啶虫脒、嘧菌环胺、吡蚜酮质量浓度4 μg·mL-1,苯醚甲环唑、氟环唑质量浓度为2 μg·mL-1,吡唑醚菌酯、丙环唑、虫酰肼、阿维菌素质量浓度为1 μg·mL-1。
1.4 样品
百合样品为药材市场采购及产地自采,共50批,其中蜜百合3批,野生百合6批,湖南百合12批,湖南陇回(自采)17批,江西百合2批,兰州百合10批。
2 拟转化百合限量标准的农药指标及范围
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GB2763-2021中收录百合2种,分别为归属药用植物类的百合(干)与归属蔬菜类的百合(鲜),二者一共覆盖12种农药信息,其中百菌清、苯醚甲环唑、吡唑醚菌酯、嘧菌环胺为GB2763.1-2022新增品种,见表1。
除草甘膦仅在鲜百合中检测外, 11种农药为干百合与鲜百合均有限量规定,存在5种农药MRL差异,且均为百合(干)高于百合(鲜),根据食品农药残留量制定原则,二者同品种农药检测方法基本一致,分析为二者干燥过程农药转移行为的原因。另外,代森锌属二硫代氨基甲酸盐,理化性质原因无法与其他农药同法共测,暂不列入本方法。根据课题组的转化原则,本方法拟转化百合(干)项下的10种农药。
3 拟转化农药的风险评估
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根据课题组的转化原则,应按照已构建的中药中农药残留风险评估体系对拟转化的农药品种进行风险评估。对百合MRL值结合《中国药典》2020年版百合项下服用量的规定6~12 g,采用公式1~4分别评价急性、慢性风险[13],结果见表2。
EXPc= E F × E d × I × M R L A T × b w
HQc=EXPc×100/ADI
其中,EXPc为慢性膳食暴露量(mg·kg-1bw·d-1);EF 为服用频率,中药饮片服用频率的P95值暂定为每年90 d;Ed为一生的暴露年限,中药饮片累积服用年限一般不超过20年;AT为平均寿命天数,以365 d×70年计;I为平均日消费量(kg·d-1),百合以药典标准平均服用量9 g计;MRL为百合中该农药的最大残留限量值(mg·kg-1);bw为平均体质量(kg),以60 kg计;HQc为慢性风险商,ADI为每日允许摄入量;100为安全因子。
EXPa= L P × M R L b w
HQA=EXPa/ARfD
其中,EXPa为急性膳食暴露量(mg·kg-1bw·d-1);LP为最大日消费量(kg·d-1),百合以药典标准12 g计;MRL为此品种中该农药的最大残留限量值(mg·kg-1);bw为平均体质量(kg),以60 kg计;HQa为急性风险商,ARfD为急性参考剂量。
结果显示,百合中11种农药的急性、慢性风险商均低于1,表明其对一般人群的急性、慢性风险处于可接受水平。
4 方法的建立与验证
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4.1 溶液制备方法
4.1.1 混合对照品溶液的制备
精密吸取10种农药混合对照品溶液1 mL,置20 mL量瓶中,用乙腈稀释至刻度,摇匀。
4.1.2 气相色谱-串联质谱法分析用内标溶液的制备
取磷酸三苯酯对照品适量,精密称定,加乙腈溶解并制成每 1 mL含1.0 mg的溶液,精密量取适量,加乙腈制成每1 mL含0.1 μg的溶液。
4.1.3 空白基质溶液的制备
取空白基质样品,同供试品溶液的制备方法处理制成空白基质溶液。
4.1.4 基质混合对照溶液的制备
分别精密量取空白基质溶液1.0 mL(6份),置氮吹仪上,40 ℃水浴浓缩至约0.4 mL,分别加入混合对照品溶液5、10、20、50、100、200、500 μL,加乙腈稀释至1 mL,涡旋混匀。
4.1.5 供试品溶液的制备
取供试品粉末(过三号筛)3 g,精密称定,置50 mL苯乙烯具塞离心管中,加入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,于冰浴中放置20 min,加入无水硫酸钠与无水乙酸钠的混合粉末(4∶1)7.5 g,立即摇散,再置振荡器上剧烈振荡(每分钟500次)3 min,离心(4 000 r·min-1)5 min。精密量取上清液1 mL,用乙腈稀释至10 mL,摇匀。
4.2 检测方法
4.2.1 液相色谱-质谱联用方法(LC-MS/MS)
色谱条件:以十八烷基硅烷键合硅胶为填充剂(2.1 mm×10 cm,1.8 μm)。以0.1%甲酸溶液(含5 mmol·L-1甲酸铵)为流动相A,以甲醇-0.1%甲酸溶液(含5 mmol·L-1甲酸铵)(95∶5)为流动相B,梯度洗脱:0~1 min,B为70%;1~12 min,B为30%→100%;12~14 min,B为100%。流速为0.3 mL·min-1,柱温为40 ℃。
质谱条件:以三重四极杆串联质谱仪检测;离子源为电喷雾(ESI)离子源,正负离子切换扫描模式。监测模式为多反应监测(MRM),各化合物参考保留时间、监测离子对、碰撞电压(CE)见表3。为提高检测灵敏度,根据保留时间分段监测各农药。
分别精密量取上述的基质混合对照溶液及供试品溶液各1 mL,精密加入水0.3 mL,混匀,滤过,取续滤液。分别精密吸取上述两种溶液各1~5 μL,注入液相色谱串联质谱仪。当供试品色谱中有相应农药检出时,取与供试品色谱峰面积最接近的对照品质量浓度,以外标法计算。
4.2.2 气相色谱-质谱联用方法(GC-MS/MS)
色谱条件:同农药残留量测定法“第五法 药材及饮片(植物类)中禁用农药多残留测定法”。
用50%苯基-甲基聚硅氧烷为固定液的弹性石英毛细管柱(柱长为30 m,柱内径为0.25 mm,膜厚度为0.25 μm)。进样口温度250 ℃,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。升温程序:初始60 ℃(保持1 min),以30 ℃·min-1升至120 ℃,再以10 ℃·min-1升至160 ℃,再以2 ℃·min-1升至230 ℃,最后再以15 ℃·min-1升至300 ℃(保持6 min)。
质谱条件: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 ℃。碰撞气为氮气或氩气。质谱传输接口温度250 ℃。质谱监测模式为MRM,各化合物参考保留时间、监测离子对、CE见表4。为提高检测灵敏度,根据保留时间分段监测各农药。
分别精密量取上述的基质混合对照溶液及供试品溶液各1 mL,精密加入内标溶液0.3 mL,混匀,滤过,取续滤液。分别精密吸取上述两种溶液各1 μL,注入气相色谱串联质谱仪。当供试品色谱中有相应农药检出时,取与供试品色谱峰面积最接近的对照品质量浓度,以内标法计算。
4.3 方法学研究
4.3.1 线性关系考察
取混合对照品溶液,精密吸取5、10、25、50、100、250、500 μL,分别置1 mL量瓶中,用乙腈稀释至刻度,配制为系列浓度溶液,精密吸取适量,测定,建立各组分的标准曲线,结果见表5,各品种在相应浓度范围内线性关系良好。
4.3.2 精密度考察
采用标准曲线第4浓度水平的溶液,连续进样6次,计算相对标准偏差(RSD)值,结果见表6,各成分在气质液质方法中精密度良好,符合痕量分析方法技术要求。
4.3.3 准确度考察
采用百合空白基质加标的方式进行低、中、高3水平回收率实验。
液质部分,分别以校准曲线最低浓度水平、第4浓度水平、最高浓度水平考察,测定结果见表6,除百菌清3水平回收率RSD值大于20%外,各成分回收率良好,回收率在72.0%~115.3%内,RSD在4.7%~12.7%内(n=9),推荐百菌清以气质方法测定,液质方法仅在必要时验证使用。
气质部分,因啶虫脒、苯醚甲环唑、丙环唑的实际信噪比不能满足最低校准浓度的灵敏度要求,采用第2浓度水平、第4浓度水平、最高浓度水平考察,其他成分以校准曲线最低浓度水平、第4浓度水平、最高浓度水平考察,测定结果见表6,各成分回收率良好,回收率在76.2%~118.9%范围内,RSD在7.6%~17.3%范围内(n=9)。
4.3.4 灵敏度考察
以校准曲线最低浓度水平的实际信噪比考察各农药品种的灵敏度,液质部分除百菌清外9个品种均大于10,气质部分除啶虫脒、苯醚甲环唑、丙环唑外3个品种均大于10。分别将各品种按准确度考察项下校准曲线最低浓度水平、第2浓度水平,将各农药相应浓度作为对应测定方法的定量下限(LLOQ),见表6,对应提取离子流图见图1。
5 样品测定结果
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按照课题组转化原则,研究所有样品为收集自市场及种植地,覆盖多产地多基源的50批百合样品,包括湖南、江西、甘肃等产地,野生百合、甘肃地方标准收载的百合及炮制品蜜百合,一定范围内确保建立方法的兼容性。采用拟定方法检测,百合中常用农药检出率相对较高,包括丙环唑、吡唑醚菌酯、苯醚甲环唑等,大多数样品的农药残留量处于较低水平,吡唑醚菌酯、苯醚甲环唑存在超标现象。各品种残留量范围、检出率、超标率见表7。
6 转化标准确定
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根据标准转化原则,基于上述标准限量和检测方法科学性、准确性验证结果,完成标准适用性评估。最终将GB2763-2021百合(干)中10种农药残留限量转化为百合药品农残限量,即百合中各农药残留量分别为百菌清(0.05 mg·kg-1)、啶虫脒(0.05 mg·kg-1)、苯醚甲环唑(0.05 mg·kg-1)、丙环唑(0.05 mg·kg-1)、吡蚜酮(0.05 mg·kg-1)、阿维菌素(0.05 mg·kg-1)、虫酰肼(0.1 mg·kg-1)、氟环唑(0.2 mg·kg-1)、吡唑醚菌酯(0.1 mg·kg-1)、嘧菌环胺(1 mg·kg-1)。
7 讨论
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7.1 空白基质及样品收集
在百合空白基质筛查中发现百合样品普遍存在监测农药检出现象,采用赴湖南龙山收集新鲜百合、野生百合等方式扩大筛查来源,得到不含监测农药(峰面积低于最低校准浓度峰面积的二分之一)的百合空白基质,空白基质、对照品及阳性样品图谱见图2。同时从市场购买百合炮制品蜜百合,增加筛查范围,为明确百合农残状况提供物质基础。
7.2 供试品溶液制备方法考察
百合中主要含有多糖、甾体皂苷、酚酸甘油酯、生物碱、黄酮等成分[14-15],供试品溶液制备针对百合基质化学成分及研究检测目标物性质,考虑中药干粉加水充分溶胀有利于提取,同时尽可能与《中国药典》2020年版禁用农残测定方法实现统一,采用《中国药典》2020年版四部通则2341第五法的QuEChERS提取方法制备。重点对百菌清、吡蚜酮分别考察酸水和水浸泡后乙腈提取的方式,10种农药中吡蚜酮、虫酰肼为使用水浸泡回收率较高,百菌清、嘧菌环胺、啶虫脒为使用酸水浸泡回收率较高,氟环唑、丙环唑、苯醚甲环唑、吡唑醚菌酯、阿维菌素2种方法条件下回收率相差不大,具体数据见表8。最终综合方法一致性、平衡采用同一方法各指标共测回收率、提高提取效率及操作便捷等原则,确定百合中转化农药品种的前处理方法。
7.3 检测方法考察
针对百合转化农药品种性质,分别采用气质联用、液质联用法考察检测条件及参数优化。其中气质法测定沸点为350 ℃的百菌清时,分别考察了不同进样口温度、传输线温度、离子源温度对结果的影响,当离子源温度为200 ℃时百菌清响应低,随着温度提升至250、290 ℃时响应值趋于稳定,结果表明在一定范围内提升温度可提高检测的灵敏度与稳定性,最终兼顾共测品种的性质,同时以与《中国药典》2020年版四部通则2341第五法气质法质谱参数尽可能统一的原则,确定检测方法。同时尝试在液质负离子模式下完成对百菌清的检测,通过优化参数可实现测定,但灵敏度及重现性等气质法测定更佳。
7.4 可共测品种方法的选择
建立液质法测定9个品种、气质法测定6个品种的方法,综合共测品种在相应方法中的灵敏度,见表6,推荐除百菌清采用气质法测定外其他9个品种均可采用液质法测定,其中嘧菌环胺、氟环唑二者均可,苯醚甲环唑、啶虫脒、丙环唑首选液质测定,共测方法可作为基质干扰或样品结果存疑的辅助验证方法。如果不能确证,可选用其他监测离子对重新进样确证或选用其他分析仪器来确证,如选用高分辨率质谱等确证手段[16]。
7.5 检测注意事项
检测过程各项操作与现行禁用农药检测法注意事项一致,如空白基质的选择、中药取样的代表性、前处理过程的控温、整体流程的控时、制备与测定的衔接、关注仪器状态、环境温湿度的影响,以确保检测数据的准确性及稳定性,同时有必要手段保证有效排除假阴性或假阳性结果[17]。
基金
收起
  • 药品监管科学全国重点实验室第一批课题(2023SKLDRS0103)
  • 国家药品监督管理局药品监管科学体系建设重点项目(RS2024Z006-110)
  • 2024年度国家药品标准制修订研究课题(2024Z01)
  • 河北省中医药管理局科研计划重点项目
文献
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参考文献 引证文献
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2024年第59卷第24期
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文章信息
doi: 10.11669/cpj.2024.24.009
  • 接收时间：2024-07-15
  • 首发时间：2025-11-13
  • 出版时间：2024-12-22
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出版历史
  • 收稿日期：2024-07-15
基金
药品监管科学全国重点实验室第一批课题(2023SKLDRS0103)
国家药品监督管理局药品监管科学体系建设重点项目(RS2024Z006-110)
2024年度国家药品标准制修订研究课题(2024Z01)
河北省中医药管理局科研计划重点项目
作者信息
    1 河北省药品医疗器械检验研究院, 国家药品监督管理局中药材质量监测评价重点实验室, 石家庄 050227
    2 中国食品药品检定研究院, 北京 102629
    3 国家药典委员会, 北京 100061

通讯作者:

* 苏建,男,硕士,正高级工程师 研究方向:中药质量及中药安全研究 Tel:(010)53852484;
马双成,男,博士,研究员 研究方向:中药质量与安全研究 Tel:(0311)69086155
参考文献
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https://castjournals.cast.org.cn/joweb/zgyxzz/CN/10.11669/cpj.2024.24.009
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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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