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Article(id=1153429495445967080, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1153429493357203682, articleNumber=null, orderNo=null, doi=10.19812/j.cnki.jfsq11-5956/ts.20240823004, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1724342400000, receivedDateStr=2024-08-23, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1752928621398, onlineDateStr=2025-07-19, pubDate=1741968000000, pubDateStr=2025-03-15, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1752928621398, onlineIssueDateStr=2025-07-19, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1752928621398, creator=13701087609, updateTime=1752928621398, updator=13701087609, issue=Issue{id=1153429493357203682, tenantId=1146029695717560320, journalId=1149652044408987649, year='2025', volume='16', issue='5', pageStart='1', pageEnd='326', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=0, createTime=1752928620900, creator=13701087609, updateTime=1758690311058, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1177595773500932351, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1153429493357203682, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1177595773500932352, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1153429493357203682, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=197, endPage=206, ext={EN=ArticleExt(id=1153429495810871531, articleId=1153429495445967080, tenantId=1146029695717560320, journalId=1149652044408987649, language=EN, title=Determination of 58 kinds of pesticide residues in animal derived food by QuEChERS-gas chromatography-tandem mass spectrometry, columnId=1153429495274000613, journalTitle=Journal of Food Safety & Quality, columnName=Special Topic: Research and Detection of Pesticide and Veterinary Drug Residue, runingTitle=null, highlight=null, articleAbstract=

Objective To establish a method for rapid determination of 58 kinds of pesticide residues in animal derived foods by QuEChERS-gas chromatography-tandem mass spectrometry (GC-MS/MS). Methods After dissolving the oil and fat in n-hexane, the sample was subjected to ultrasonic extraction with a saturated acetonitrile solution (containing 1% glacial acetic acid). The extract was purified with anhydrous magnesium sulfate, octadecyl bonded silica gel (C18), and N-propylethylenediamine (PSA), and then nitrogen was blown to near dryness in a water bath. An internal standard was added and dissolved in ethyl acetate. GC-MS/MS was used for determination, and the blank matrix matching standard curve internal standard method was used for quantification. Results The linear relationship between 58 kinds of pesticides was good within the mass concentration range of 0.005-0.500 mg/L, with correlation coefficients (r2) greater than 0.9945. The limits of detection and limits of quantification were 0.001-0.005 mg/kg and 0.002-0.015 mg/kg, respectively. The average recovery rates of pork, chicken, fish, eggs and milk matrices at 3 different spiked levels ranged from 71.8% to 117.4%, with relative standard deviations of 0.7% to 8.7% (n=4). Conclusion This method has high sensitivity and good accuracy, and is suitable for simultaneous determination of 58 kinds of pesticide residues in animal derived foods.

, correspAuthors=Kai YANG, 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=Kai YANG, Li-Ping SUN, Yan OUYANG), CN=ArticleExt(id=1153429519177339589, articleId=1153429495445967080, tenantId=1146029695717560320, journalId=1149652044408987649, language=CN, title=QuEChERS-气相色谱-串联质谱法测定动物源性食品中58种农药残留量, columnId=1153429495479521513, journalTitle=食品安全质量检测学报, columnName=本期专题：农兽药残留研究与检测, runingTitle=null, highlight=null, articleAbstract=

目的 建立QuEChERS-气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry, GC-MS/MS)同时快速测定动物源性食品中58种农药残留的分析方法。方法 样品用正己烷溶解油脂后, 加入正己烷饱和乙腈(含1%冰醋酸)溶液超声提取, 提取液经无水硫酸镁、十八烷基键合硅胶(C18)和N-丙基乙二胺(N-propylethylenediamine, PSA)净化后水浴氮吹至近干, 加入内标并用乙酸乙酯复溶。采用GC-MS/MS测定, 空白基质匹配标准曲线内标法定量。结果 58种农药在0.005~0.500 mg/L质量浓度范围内线性关系良好, 相关系数(r2)均大于0.9945, 检出限和定量限分别为0.001~0.005 mg/kg和0.002~0.015 mg/kg。在猪肉、鸡肉、鱼肉、鸡蛋和牛奶5种基质中, 3个不同加标水平下的平均回收率为71.8%~117.4%, 相对标准偏差为0.7%~8.7% (n=4)。结论 该方法灵敏度高、准确性好, 适用于动物源性食品中58种农药残留的同时测定。

, correspAuthors=杨凯, authorNote=null, correspAuthorsNote=
* 杨凯(1987—), 男, 硕士, 农艺师, 主要研究方向为农产品质量安全监测。E-mail:
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Journal of Instrumental Analysis, 2022, 41(8): 1221-1228., articleTitle=Determination of 37 kinds of pesticide residues in tea by gas chromatography-tandem mass spectrometry combined with QuEChERS and prepositive internal standard, refAbstract=null)], funds=null, companyList=[AuthorCompany(id=1177619572879410129, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153429495445967080, xref=null, ext=[AuthorCompanyExt(id=1177619572908770258, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153429495445967080, companyId=1177619572879410129, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=Shenzhen Agricultural Product Quality and Safety Inspection and Testing Center, Shenzhen 518055, China), AuthorCompanyExt(id=1177619572929741779, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153429495445967080, companyId=1177619572879410129, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=深圳市农产品质量安全检验检测中心, 深圳 518055)])], figs=[ArticleFig(id=1177619574980756474, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153429495445967080, language=EN, label=Fig.1, caption=Total ion chromatogram of 58 kinds of pesticides in pork blank matrix matching standard solution (0.500 mg/L), figureFileSmall=Q5i2Rp8+uUyZcqy5Z5PEpw==, figureFileBig=vdCmfYHEISFt5vL9PCT+nA==, tableContent=null), ArticleFig(id=1177619575031088124, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153429495445967080, language=CN, label=图1, caption=58种农药在猪肉空白基质匹配标准溶液(0.500 mg/L)中的总离子流色谱图, figureFileSmall=Q5i2Rp8+uUyZcqy5Z5PEpw==, figureFileBig=vdCmfYHEISFt5vL9PCT+nA==, tableContent=null), ArticleFig(id=1177619575094002686, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153429495445967080, language=EN, label=Fig.2, caption=Recoveries of 58 kinds of pesticides extracted with different solvents, figureFileSmall=Vd9JFHZIkcFw8k78nRUjGw==, figureFileBig=nTRU3/81q5cGY6h0ipkLkw==, tableContent=null), ArticleFig(id=1177619575148528640, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153429495445967080, language=CN, label=图2, caption=不同溶剂提取58种农药的回收率, figureFileSmall=Vd9JFHZIkcFw8k78nRUjGw==, figureFileBig=nTRU3/81q5cGY6h0ipkLkw==, tableContent=null), ArticleFig(id=1177619575194664961, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153429495445967080, language=EN, label=Fig.3, caption=Effects of 3 types of salt packs on the recovery rates of 58 kinds of pesticides, figureFileSmall=+zuuw3F9tXoLjv55NQf5Jg==, figureFileBig=CfGgu6Mi2+fdytu0tibWoA==, tableContent=null), ArticleFig(id=1177619575249190915, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153429495445967080, language=CN, label=图3, caption=3种盐包对58种农药回收率的影响, figureFileSmall=+zuuw3F9tXoLjv55NQf5Jg==, figureFileBig=CfGgu6Mi2+fdytu0tibWoA==, tableContent=null), ArticleFig(id=1177619575395991557, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153429495445967080, language=EN, label=Fig.4, caption=Effects of different freezing times on the recovery rates of 58 kinds of pesticides, figureFileSmall=BpRiE82/mmt/DVL1NpvRhA==, figureFileBig=pQ77CLRPKS4emonRhl2cog==, tableContent=null), ArticleFig(id=1177619575463100423, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153429495445967080, language=CN, label=图4, caption=不同冷冻时间对58种农药回收率的影响, figureFileSmall=BpRiE82/mmt/DVL1NpvRhA==, figureFileBig=pQ77CLRPKS4emonRhl2cog==, tableContent=null), ArticleFig(id=1177619575534403593, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153429495445967080, language=EN, label=Fig.5, caption=MEs of 58 kinds of pesticides in different animal derived foods, figureFileSmall=y8lW8viw3m2JwaayVWUwmw==, figureFileBig=BsJnFm2Uj3baxRRaVhQ9xg==, tableContent=null), ArticleFig(id=1177619575609901066, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153429495445967080, language=CN, label=图5, caption=58种农药在不同动物源性食品中的MEs, figureFileSmall=y8lW8viw3m2JwaayVWUwmw==, figureFileBig=BsJnFm2Uj3baxRRaVhQ9xg==, tableContent=null), ArticleFig(id=1177619575672815628, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153429495445967080, language=EN, label=Table 1, caption=

Mass spectrometry parameters of 58 kinds of pesticides and internal standard

, figureFileSmall=null, figureFileBig=null, tableContent=
序号 农药名称 保留时间/min 定性离子对(m/z) 定量离子对(m/z) 碰撞能量/eV
1 甲胺磷 3.70 141.00/79.00 141.00/94.80 20, 6
2 敌敌畏 3.72 185.00/93.00 109.00/79.00 12, 6
3 乙酰甲胺磷 4.82 136.00/94.00 136.00/42.10 12, 8
4 氧乐果 6.28 109.80/79.00 156.00/110.00 11, 8
5 甲拌磷 7.07 75.00/47.00 121.00/65.00 8, 8
6 α-六六六 7.22 216.90/181.00 182.80/146.70 8, 12
7 乐果 7.44 93.00/63.00 87.00/42.10 8, 8
8 克百威 7.48 149.10/77.00 164.00/149.10 24, 8
9 β-六六六 7.70 216.90/181.00 180.90/145.00 8, 14
10 五氯硝基苯 7.76 213.80/141.90 213.80/178.90 28, 12
11 γ-六六六 7.86 218.70/183.00 180.90/145.00 8, 14
12 二嗪磷 7.96 137.10/54.10 137.10/84.10 20, 12
13 嘧霉胺 8.13 198.10/117.90 198.10/182.90 30, 14
14 氯唑磷 8.13 198.10/157.60 198.10/117.90 18, 8
15 δ-六六六 8.40 218.80/182.90 181.00/145.00 8, 13
16 氟甲腈 8.98 333.00/231.00 388.00/333.10 23, 15
17 乙烯菌核利 9.02 198.00/145.00 186.80/124.00 14, 16
18 甲基对硫磷 9.08 124.90/47.00 124.90/79.00 12, 6
19 甲霜灵 9.23 131.90/117.00 234.00/146.00 12, 18
20 甲萘威 9.26 144.00/116.00 144.00/115.00 11, 22
21 杀螟硫磷 9.57 125.00/79.00 277.00/260.00 8, 6
22 马拉硫磷 9.74 125.00/79.00 127.00/99.00 8, 8
23 毒死蜱 9.92 199.00/171.00 196.70/168.90 5, 10
24 对硫磷 10.12 291.00/109.00 109.00/81.00 6, 8
25 三唑酮 10.20 208.00/111.00 208.00/180.80 18, 8
26 水胺硫磷 10.23 121.10/65.00 136.00/108.00 14, 12
27 三氯杀螨醇 10.34 111.00/74.90 139.00/111.00 12, 12
28 氟虫腈硫醚 10.56 419.80/351.10 351.00/255.00 10, 30
29 甲基异柳磷 10.56 241.10/121.10 199.00/121.00 20, 10
30 二甲戊灵 10.67 252.10/161.00 252.10/162.00 14, 8
31 氟虫腈 10.75 368.80/214.90 366.90/212.90 28, 28
32 硫环磷 10.98 195.80/139.90 168.00/140.00 10, 8
33 三唑醇 11.07 128.00/65.00 168.20/70.00 18, 8
34 多效唑 11.39 236.00/167.00 236.00/125.00 8, 18
35 氟啶脲 11.52 322.88/306.14 320.91/304.05 30, 20
36 氟虫腈砜 11.79 383.00/241.00 383.00/255.00 10, 17
37 丙溴磷 11.76 336.90/266.90 339.00/268.90 6, 15
38 虫螨腈 12.01 137.10/102.00 247.10/227.00 12, 15
39 三唑磷 12.51 162.10/119.10 161.00/134.10 8, 10
40 丙环唑 12.79 172.90/109.00 172.90/145.00 24, 14
41 戊唑醇 13.00 125.00/89.00 250.00/125.00 16, 20
42 联苯菊酯 13.39 181.00/165.20 181.00/165.90 21, 10
43 亚胺硫磷 13.45 160.00/133.00 160.00/76.90 10, 22
44 甲氰菊酯 13.55 264.90/210.00 181.00/151.90 10, 20
45 伏杀硫磷 13.98 182.00/74.80 182.00/111.00 30, 12
46 氯氟氰菊酯 14.19 197.10/141.10 207.90/180.90 10, 8
47 氯菊酯 15.17 183.10/153.00 183.10/168.00 12, 12
48 哒螨灵 15.26 147.10/132.10 147.10/117.10 12, 20
49 氟氯氰菊酯 15.93 226.00/206.10 163.00/91.10 12, 12
50 氯氰菊酯 16.25 180.90/152.10 163.00/91.10 20, 12
51 氟氰戊菊酯 16.41 199.10/157.10 157.00/107.10 8, 20
52 醚菊酯 16.59 163.10/135.10 163.10/107.10 8, 16
53 氰戊菊酯 17.70 125.00/89.00 167.00/125.00 26, 10
54 氟胺氰菊酯 17.77 180.80/152.10 250.00/55.10 20, 14
55 吡唑醚菌酯 17.78 164.00/132.10 132.00/77.00 8, 19
56 苯醚甲环唑 18.60 265.00/139.00 323.00/265.00 40, 16
57 溴氰菊酯 18.67 252.80/92.90 181.00/152.10 18, 18
58 醚菌酯 19.49 344.10/156.00 344.10/329.00 34, 12
内标 环氧七氯A 10.97 183.00/155.00 135.00/99.00 11, 9
), ArticleFig(id=1177619575781867534, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153429495445967080, language=CN, label=表1, caption=

58种农药及内标的质谱参数

, figureFileSmall=null, figureFileBig=null, tableContent=
序号 农药名称 保留时间/min 定性离子对(m/z) 定量离子对(m/z) 碰撞能量/eV
1 甲胺磷 3.70 141.00/79.00 141.00/94.80 20, 6
2 敌敌畏 3.72 185.00/93.00 109.00/79.00 12, 6
3 乙酰甲胺磷 4.82 136.00/94.00 136.00/42.10 12, 8
4 氧乐果 6.28 109.80/79.00 156.00/110.00 11, 8
5 甲拌磷 7.07 75.00/47.00 121.00/65.00 8, 8
6 α-六六六 7.22 216.90/181.00 182.80/146.70 8, 12
7 乐果 7.44 93.00/63.00 87.00/42.10 8, 8
8 克百威 7.48 149.10/77.00 164.00/149.10 24, 8
9 β-六六六 7.70 216.90/181.00 180.90/145.00 8, 14
10 五氯硝基苯 7.76 213.80/141.90 213.80/178.90 28, 12
11 γ-六六六 7.86 218.70/183.00 180.90/145.00 8, 14
12 二嗪磷 7.96 137.10/54.10 137.10/84.10 20, 12
13 嘧霉胺 8.13 198.10/117.90 198.10/182.90 30, 14
14 氯唑磷 8.13 198.10/157.60 198.10/117.90 18, 8
15 δ-六六六 8.40 218.80/182.90 181.00/145.00 8, 13
16 氟甲腈 8.98 333.00/231.00 388.00/333.10 23, 15
17 乙烯菌核利 9.02 198.00/145.00 186.80/124.00 14, 16
18 甲基对硫磷 9.08 124.90/47.00 124.90/79.00 12, 6
19 甲霜灵 9.23 131.90/117.00 234.00/146.00 12, 18
20 甲萘威 9.26 144.00/116.00 144.00/115.00 11, 22
21 杀螟硫磷 9.57 125.00/79.00 277.00/260.00 8, 6
22 马拉硫磷 9.74 125.00/79.00 127.00/99.00 8, 8
23 毒死蜱 9.92 199.00/171.00 196.70/168.90 5, 10
24 对硫磷 10.12 291.00/109.00 109.00/81.00 6, 8
25 三唑酮 10.20 208.00/111.00 208.00/180.80 18, 8
26 水胺硫磷 10.23 121.10/65.00 136.00/108.00 14, 12
27 三氯杀螨醇 10.34 111.00/74.90 139.00/111.00 12, 12
28 氟虫腈硫醚 10.56 419.80/351.10 351.00/255.00 10, 30
29 甲基异柳磷 10.56 241.10/121.10 199.00/121.00 20, 10
30 二甲戊灵 10.67 252.10/161.00 252.10/162.00 14, 8
31 氟虫腈 10.75 368.80/214.90 366.90/212.90 28, 28
32 硫环磷 10.98 195.80/139.90 168.00/140.00 10, 8
33 三唑醇 11.07 128.00/65.00 168.20/70.00 18, 8
34 多效唑 11.39 236.00/167.00 236.00/125.00 8, 18
35 氟啶脲 11.52 322.88/306.14 320.91/304.05 30, 20
36 氟虫腈砜 11.79 383.00/241.00 383.00/255.00 10, 17
37 丙溴磷 11.76 336.90/266.90 339.00/268.90 6, 15
38 虫螨腈 12.01 137.10/102.00 247.10/227.00 12, 15
39 三唑磷 12.51 162.10/119.10 161.00/134.10 8, 10
40 丙环唑 12.79 172.90/109.00 172.90/145.00 24, 14
41 戊唑醇 13.00 125.00/89.00 250.00/125.00 16, 20
42 联苯菊酯 13.39 181.00/165.20 181.00/165.90 21, 10
43 亚胺硫磷 13.45 160.00/133.00 160.00/76.90 10, 22
44 甲氰菊酯 13.55 264.90/210.00 181.00/151.90 10, 20
45 伏杀硫磷 13.98 182.00/74.80 182.00/111.00 30, 12
46 氯氟氰菊酯 14.19 197.10/141.10 207.90/180.90 10, 8
47 氯菊酯 15.17 183.10/153.00 183.10/168.00 12, 12
48 哒螨灵 15.26 147.10/132.10 147.10/117.10 12, 20
49 氟氯氰菊酯 15.93 226.00/206.10 163.00/91.10 12, 12
50 氯氰菊酯 16.25 180.90/152.10 163.00/91.10 20, 12
51 氟氰戊菊酯 16.41 199.10/157.10 157.00/107.10 8, 20
52 醚菊酯 16.59 163.10/135.10 163.10/107.10 8, 16
53 氰戊菊酯 17.70 125.00/89.00 167.00/125.00 26, 10
54 氟胺氰菊酯 17.77 180.80/152.10 250.00/55.10 20, 14
55 吡唑醚菌酯 17.78 164.00/132.10 132.00/77.00 8, 19
56 苯醚甲环唑 18.60 265.00/139.00 323.00/265.00 40, 16
57 溴氰菊酯 18.67 252.80/92.90 181.00/152.10 18, 18
58 醚菌酯 19.49 344.10/156.00 344.10/329.00 34, 12
内标 环氧七氯A 10.97 183.00/155.00 135.00/99.00 11, 9
), ArticleFig(id=1177619575865753616, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153429495445967080, language=EN, label=Table 2, caption=

Linear ranges, linear equations, correlation coefficients, limits of detection and limits of quantification of 58 kinds of pesticides

, figureFileSmall=null, figureFileBig=null, tableContent=
序号 农药名称 线性范围/(mg/L) 线性方程 相关系数(r2) 检出限/(mg/kg) 定量限/(mg/kg)
1 甲胺磷 0.005~0.500 Y=493X+1 0.9984 0.003 0.010
2 敌敌畏 0.005~0.500 Y=1328X+1 0.9996 0.001 0.004
3 乙酰甲胺磷 0.005~0.500 Y=380X-1 0.9980 0.003 0.010
4 氧乐果 0.005~0.500 Y=395X+2 0.9945 0.003 0.010
5 甲拌磷 0.005~0.500 Y=2066X+3 0.9992 0.001 0.003
6 α-六六六 0.005~0.500 Y=1087X 0.9997 0.001 0.004
7 乐果 0.005~0.500 Y=1385X+3 0.9996 0.005 0.015
8 克百威 0.005~0.500 Y=467X+15 0.9948 0.004 0.015
9 β-六六六 0.005~0.500 Y=2786X-5 0.9996 0.003 0.010
10 五氯硝基苯 0.005~0.500 Y=673X-1 0.9991 0.005 0.015
11 γ-六六六 0.005~0.500 Y=2785X-5 0.9996 0.003 0.010
12 二嗪磷 0.005~0.500 Y=1147X+1 0.9995 0.001 0.004
13 嘧霉胺 0.005~0.500 Y=1935X+6 0.9994 0.001 0.005
14 氯唑磷 0.005~0.500 Y=1564X 0.9995 0.005 0.015
15 δ-六六六 0.005~0.500 Y=626X 0.9995 0.004 0.015
16 氟甲腈 0.005~0.500 Y=2043X+4 0.9997 0.005 0.015
17 乙烯菌核利 0.005~0.500 Y=885X-1 0.9993 0.005 0.015
18 甲基对硫磷 0.005~0.500 Y=699X+6 0.9998 0.005 0.015
19 甲霜灵 0.005~0.500 Y=1080X+4 0.9985 0.001 0.003
20 甲萘威 0.005~0.500 Y=1209X+8 0.9958 0.005 0.015
21 杀螟硫磷 0.005~0.500 Y=953X-2 0.9999 0.005 0.015
22 马拉硫磷 0.005~0.500 Y=2450X+30 0.9993 0.001 0.002
23 毒死蜱 0.005~0.500 Y=1528X+3 0.9993 0.001 0.004
24 对硫磷 0.005~0.500 Y=1353X+16 0.9979 0.005 0.015
25 三唑酮 0.005~0.500 Y=1072X 0.9997 0.002 0.006
26 水胺硫磷 0.005~0.500 Y=3149X+13 0.9995 0.002 0.006
27 三氯杀螨醇 0.005~0.500 Y=6192X+13 0.9994 0.001 0.002
28 氟甲腈硫醚 0.005~0.500 Y=4335X+11 0.9993 0.005 0.015
29 甲基异柳磷 0.005~0.500 Y=5449X+9 0.9993 0.001 0.002
30 二甲戊灵 0.005~0.500 Y=1044X-2 0.9993 0.001 0.005
31 氟虫腈 0.005~0.500 Y=2162X-1 0.9997 0.001 0.004
32 硫环磷 0.005~0.500 Y=1383X 0.9994 0.005 0.015
33 三唑醇 0.005~0.500 Y=1463X+7 0.9991 0.002 0.006
34 多效唑 0.005~0.500 Y=3420X+12 0.9993 0.001 0.002
35 氟啶脲 0.005~0.500 Y=1036X-2 0.9991 0.002 0.007
36 氟虫腈砜 0.005~0.500 Y=3198X+7 0.9990 0.001 0.002
37 丙溴磷 0.005~0.500 Y=887X+2 0.9997 0.001 0.004
38 虫螨腈 0.005~0.500 Y=128X 0.9982 0.005 0.015
39 三唑磷 0.005~0.500 Y=1253X+2 0.9995 0.001 0.004
40 丙环唑 0.005~0.500 Y=2954X+23 0.9994 0.005 0.015
41 戊唑醇 0.005~0.500 Y=2240X+6 0.9986 0.001 0.002
42 联苯菊酯 0.005~0.500 Y=12354X+27 0.9995 0.001 0.002
43 亚胺硫磷 0.005~0.500 Y=1618X+6 0.9986 0.002 0.006
44 甲氰菊酯 0.005~0.500 Y=1926X+6 0.9988 0.001 0.004
45 伏杀硫磷 0.005~0.500 Y=2269X+8 0.9997 0.002 0.007
46 氯氟氰菊酯 0.005~0.500 Y=1609X+5 0.9993 0.005 0.015
47 氯菊酯 0.005~0.500 Y=1740X+11 0.9989 0.005 0.015
48 哒螨灵 0.005~0.500 Y=8893X+24 0.9992 0.001 0.002
49 氟氯氰菊酯 0.005~0.500 Y=893X+2 0.9994 0.005 0.015
50 氯氰菊酯 0.005~0.500 Y=1332X+2 0.9994 0.005 0.015
51 氟氰戊菊酯 0.005~0.500 Y=3247X+12 0.9992 0.005 0.015
52 醚菊酯 0.005~0.500 Y=9838X+15 0.9995 0.003 0.009
53 氰戊菊酯 0.005~0.500 Y=2317X 0.9995 0.003 0.009
54 氟胺氰菊酯 0.005~0.500 Y=501X+2 0.9983 0.005 0.015
55 吡唑醚菌酯 0.005~0.500 Y=2640X+6 0.9996 0.005 0.015
56 苯醚甲环唑 0.005~0.500 Y=8671X+32 0.9988 0.001 0.003
57 溴氰菊酯 0.005~0.500 Y=851X-2 0.9987 0.004 0.013
58 醚菌酯 0.005~0.500 Y=3059X+13 0.9989 0.001 0.002
), ArticleFig(id=1177619575978999826, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153429495445967080, language=CN, label=表2, caption=

58种农药的线性范围、线性方程、相关系数、检出限与定量限

, figureFileSmall=null, figureFileBig=null, tableContent=
序号 农药名称 线性范围/(mg/L) 线性方程 相关系数(r2) 检出限/(mg/kg) 定量限/(mg/kg)
1 甲胺磷 0.005~0.500 Y=493X+1 0.9984 0.003 0.010
2 敌敌畏 0.005~0.500 Y=1328X+1 0.9996 0.001 0.004
3 乙酰甲胺磷 0.005~0.500 Y=380X-1 0.9980 0.003 0.010
4 氧乐果 0.005~0.500 Y=395X+2 0.9945 0.003 0.010
5 甲拌磷 0.005~0.500 Y=2066X+3 0.9992 0.001 0.003
6 α-六六六 0.005~0.500 Y=1087X 0.9997 0.001 0.004
7 乐果 0.005~0.500 Y=1385X+3 0.9996 0.005 0.015
8 克百威 0.005~0.500 Y=467X+15 0.9948 0.004 0.015
9 β-六六六 0.005~0.500 Y=2786X-5 0.9996 0.003 0.010
10 五氯硝基苯 0.005~0.500 Y=673X-1 0.9991 0.005 0.015
11 γ-六六六 0.005~0.500 Y=2785X-5 0.9996 0.003 0.010
12 二嗪磷 0.005~0.500 Y=1147X+1 0.9995 0.001 0.004
13 嘧霉胺 0.005~0.500 Y=1935X+6 0.9994 0.001 0.005
14 氯唑磷 0.005~0.500 Y=1564X 0.9995 0.005 0.015
15 δ-六六六 0.005~0.500 Y=626X 0.9995 0.004 0.015
16 氟甲腈 0.005~0.500 Y=2043X+4 0.9997 0.005 0.015
17 乙烯菌核利 0.005~0.500 Y=885X-1 0.9993 0.005 0.015
18 甲基对硫磷 0.005~0.500 Y=699X+6 0.9998 0.005 0.015
19 甲霜灵 0.005~0.500 Y=1080X+4 0.9985 0.001 0.003
20 甲萘威 0.005~0.500 Y=1209X+8 0.9958 0.005 0.015
21 杀螟硫磷 0.005~0.500 Y=953X-2 0.9999 0.005 0.015
22 马拉硫磷 0.005~0.500 Y=2450X+30 0.9993 0.001 0.002
23 毒死蜱 0.005~0.500 Y=1528X+3 0.9993 0.001 0.004
24 对硫磷 0.005~0.500 Y=1353X+16 0.9979 0.005 0.015
25 三唑酮 0.005~0.500 Y=1072X 0.9997 0.002 0.006
26 水胺硫磷 0.005~0.500 Y=3149X+13 0.9995 0.002 0.006
27 三氯杀螨醇 0.005~0.500 Y=6192X+13 0.9994 0.001 0.002
28 氟甲腈硫醚 0.005~0.500 Y=4335X+11 0.9993 0.005 0.015
29 甲基异柳磷 0.005~0.500 Y=5449X+9 0.9993 0.001 0.002
30 二甲戊灵 0.005~0.500 Y=1044X-2 0.9993 0.001 0.005
31 氟虫腈 0.005~0.500 Y=2162X-1 0.9997 0.001 0.004
32 硫环磷 0.005~0.500 Y=1383X 0.9994 0.005 0.015
33 三唑醇 0.005~0.500 Y=1463X+7 0.9991 0.002 0.006
34 多效唑 0.005~0.500 Y=3420X+12 0.9993 0.001 0.002
35 氟啶脲 0.005~0.500 Y=1036X-2 0.9991 0.002 0.007
36 氟虫腈砜 0.005~0.500 Y=3198X+7 0.9990 0.001 0.002
37 丙溴磷 0.005~0.500 Y=887X+2 0.9997 0.001 0.004
38 虫螨腈 0.005~0.500 Y=128X 0.9982 0.005 0.015
39 三唑磷 0.005~0.500 Y=1253X+2 0.9995 0.001 0.004
40 丙环唑 0.005~0.500 Y=2954X+23 0.9994 0.005 0.015
41 戊唑醇 0.005~0.500 Y=2240X+6 0.9986 0.001 0.002
42 联苯菊酯 0.005~0.500 Y=12354X+27 0.9995 0.001 0.002
43 亚胺硫磷 0.005~0.500 Y=1618X+6 0.9986 0.002 0.006
44 甲氰菊酯 0.005~0.500 Y=1926X+6 0.9988 0.001 0.004
45 伏杀硫磷 0.005~0.500 Y=2269X+8 0.9997 0.002 0.007
46 氯氟氰菊酯 0.005~0.500 Y=1609X+5 0.9993 0.005 0.015
47 氯菊酯 0.005~0.500 Y=1740X+11 0.9989 0.005 0.015
48 哒螨灵 0.005~0.500 Y=8893X+24 0.9992 0.001 0.002
49 氟氯氰菊酯 0.005~0.500 Y=893X+2 0.9994 0.005 0.015
50 氯氰菊酯 0.005~0.500 Y=1332X+2 0.9994 0.005 0.015
51 氟氰戊菊酯 0.005~0.500 Y=3247X+12 0.9992 0.005 0.015
52 醚菊酯 0.005~0.500 Y=9838X+15 0.9995 0.003 0.009
53 氰戊菊酯 0.005~0.500 Y=2317X 0.9995 0.003 0.009
54 氟胺氰菊酯 0.005~0.500 Y=501X+2 0.9983 0.005 0.015
55 吡唑醚菌酯 0.005~0.500 Y=2640X+6 0.9996 0.005 0.015
56 苯醚甲环唑 0.005~0.500 Y=8671X+32 0.9988 0.001 0.003
57 溴氰菊酯 0.005~0.500 Y=851X-2 0.9987 0.004 0.013
58 醚菌酯 0.005~0.500 Y=3059X+13 0.9989 0.001 0.002
), ArticleFig(id=1177619576058691604, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153429495445967080, language=EN, label=Table 3, caption=

Spiked recovery rates and relative standard deviations of 58 kinds of pesticides (n=4)

, figureFileSmall=null, figureFileBig=null, tableContent=
基质 添加含量/(mg/kg) 回收率/% 相对标准
偏差/%
猪肉 0.02 75.3~106.7 0.8~6.5
0.05 75.2~112.6 1.3~5.7
0.20 83.6~103.8 1.1~4.8
鸡肉 0.02 72.6~112.4 1.6~7.3
0.05 81.7~109.2 2.4~5.5
0.20 88.3~105.3 2.1~5.2
鱼肉 0.02 75.8~117.4 0.8~6.6
0.05 79.5~112.2 1.7~4.9
0.20 83.3~106.4 1.3~7.0
鸡蛋 0.02 76.8~99.7 2.3~8.7
0.05 71.8~115.2 1.5~5.8
0.20 82.5~104.5 1.4~4.9
牛奶 0.02 76.6~107.2 0.9~4.6
0.05 75.2~114.5 1.2~4.9
0.20 85.5~106.8 0.7~3.3
), ArticleFig(id=1177619576150966294, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153429495445967080, language=CN, label=表3, caption=

58种农药的加标回收率和相对标准偏差(n=4)

, figureFileSmall=null, figureFileBig=null, tableContent=
基质 添加含量/(mg/kg) 回收率/% 相对标准
偏差/%
猪肉 0.02 75.3~106.7 0.8~6.5
0.05 75.2~112.6 1.3~5.7
0.20 83.6~103.8 1.1~4.8
鸡肉 0.02 72.6~112.4 1.6~7.3
0.05 81.7~109.2 2.4~5.5
0.20 88.3~105.3 2.1~5.2
鱼肉 0.02 75.8~117.4 0.8~6.6
0.05 79.5~112.2 1.7~4.9
0.20 83.3~106.4 1.3~7.0
鸡蛋 0.02 76.8~99.7 2.3~8.7
0.05 71.8~115.2 1.5~5.8
0.20 82.5~104.5 1.4~4.9
牛奶 0.02 76.6~107.2 0.9~4.6
0.05 75.2~114.5 1.2~4.9
0.20 85.5~106.8 0.7~3.3
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QuEChERS-气相色谱-串联质谱法测定动物源性食品中58种农药残留量
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杨凯 * , 孙丽萍 , 欧阳燕
食品安全质量检测学报 | 本期专题：农兽药残留研究与检测 2025,16(5): 197-206
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食品安全质量检测学报 | 本期专题：农兽药残留研究与检测 2025, 16(5): 197-206
QuEChERS-气相色谱-串联质谱法测定动物源性食品中58种农药残留量
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杨凯* , 孙丽萍, 欧阳燕
作者信息
  • 深圳市农产品质量安全检验检测中心, 深圳 518055

通讯作者:

* 杨凯(1987—), 男, 硕士, 农艺师, 主要研究方向为农产品质量安全监测。E-mail:
Determination of 58 kinds of pesticide residues in animal derived food by QuEChERS-gas chromatography-tandem mass spectrometry
Kai YANG* , Li-Ping SUN, Yan OUYANG
Affiliations
  • Shenzhen Agricultural Product Quality and Safety Inspection and Testing Center, Shenzhen 518055, China
出版时间: 2025-03-15 doi: 10.19812/j.cnki.jfsq11-5956/ts.20240823004
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摘要
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目的 建立QuEChERS-气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry, GC-MS/MS)同时快速测定动物源性食品中58种农药残留的分析方法。方法 样品用正己烷溶解油脂后, 加入正己烷饱和乙腈(含1%冰醋酸)溶液超声提取, 提取液经无水硫酸镁、十八烷基键合硅胶(C18)和N-丙基乙二胺(N-propylethylenediamine, PSA)净化后水浴氮吹至近干, 加入内标并用乙酸乙酯复溶。采用GC-MS/MS测定, 空白基质匹配标准曲线内标法定量。结果 58种农药在0.005~0.500 mg/L质量浓度范围内线性关系良好, 相关系数(r2)均大于0.9945, 检出限和定量限分别为0.001~0.005 mg/kg和0.002~0.015 mg/kg。在猪肉、鸡肉、鱼肉、鸡蛋和牛奶5种基质中, 3个不同加标水平下的平均回收率为71.8%~117.4%, 相对标准偏差为0.7%~8.7% (n=4)。结论 该方法灵敏度高、准确性好, 适用于动物源性食品中58种农药残留的同时测定。

QuEChERS  /  气相色谱-串联质谱法  /  动物源性食品  /  农药残留

Objective To establish a method for rapid determination of 58 kinds of pesticide residues in animal derived foods by QuEChERS-gas chromatography-tandem mass spectrometry (GC-MS/MS). Methods After dissolving the oil and fat in n-hexane, the sample was subjected to ultrasonic extraction with a saturated acetonitrile solution (containing 1% glacial acetic acid). The extract was purified with anhydrous magnesium sulfate, octadecyl bonded silica gel (C18), and N-propylethylenediamine (PSA), and then nitrogen was blown to near dryness in a water bath. An internal standard was added and dissolved in ethyl acetate. GC-MS/MS was used for determination, and the blank matrix matching standard curve internal standard method was used for quantification. Results The linear relationship between 58 kinds of pesticides was good within the mass concentration range of 0.005-0.500 mg/L, with correlation coefficients (r2) greater than 0.9945. The limits of detection and limits of quantification were 0.001-0.005 mg/kg and 0.002-0.015 mg/kg, respectively. The average recovery rates of pork, chicken, fish, eggs and milk matrices at 3 different spiked levels ranged from 71.8% to 117.4%, with relative standard deviations of 0.7% to 8.7% (n=4). Conclusion This method has high sensitivity and good accuracy, and is suitable for simultaneous determination of 58 kinds of pesticide residues in animal derived foods.

QuEChERS  /  gas chromatography-tandem mass spectrometry  /  animal derived food  /  pesticide residue
杨凯, 孙丽萍, 欧阳燕. QuEChERS-气相色谱-串联质谱法测定动物源性食品中58种农药残留量. 食品安全质量检测学报, 2025 , 16 (5) : 197 -206 . DOI: 10.19812/j.cnki.jfsq11-5956/ts.20240823004
Kai YANG, Li-Ping SUN, Yan OUYANG. Determination of 58 kinds of pesticide residues in animal derived food by QuEChERS-gas chromatography-tandem mass spectrometry[J]. Journal of Food Safety & Quality, 2025 , 16 (5) : 197 -206 . DOI: 10.19812/j.cnki.jfsq11-5956/ts.20240823004
正文
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0 引言
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动物源性食品, 如肉类、蛋类、奶制品等, 是人们饮食的重要组成部分。这些食品在生产、加工和储运过程中可能会接触到各种农药, 尽管动物源性食品中的农药残留量一般较低, 但由于大部分动物源性食品属于日常使用的生活必需品, 在长期低剂量暴露于农药及其代谢物的情况下, 可能导致人体生殖毒性及神经毒性等潜在安全风险[1]。目前国内外对农药残留检测的相关研究主要针对的是植物源性食品, 如蔬菜[2-4]、水果[5-7]、药材[8-10]等, 有关动物源性食品中农药残留的研究[11-13]相对较少, 动物源性食品中农药残留的国家/行业检测标准往往针对少数几种或某一类(如有机磷、有机氯或菊酯类等)农药。近年来, 国家越来越重视动物源性食品中的农药残留问题, 制定的标准对动物源性食品中农药残留限量的规定日趋严格。因此, 亟需开展动物源性食品中农药残留检测方法的相关研究, 确保动物源性食品的质量安全和消费者身体健康。
动物源性食品中含有脂肪、色素、蛋白质、磷脂、糖类等干扰成分, 减少或消除从样品基质中提取农药过程中的干扰成分是分析实验的关键。QuEChERS法是ANASTASSIADES等在2003年研发的一种提取和净化于一体的农药残留检测样品前处理技术, 该方法以乙腈为提取试剂, 盐析去除乙腈中混合的水分, 然后用N-丙基乙二胺(N-propylethylenediamine, PSA)和无水硫酸镁去除提取液中的杂质和水分, 具有快速、简便、廉价、高效、可靠、安全的优点[14-15]。QuEChERS法适用性极强, 不仅适用于植物源性食品中农药残留的提取和净化, 也适用于动物性食品中农药残留的提取和净化[16-17]。气相色谱-串联质谱法(gas chromatography tandem mass spectrometry, GC-MS/MS)采用二级离子定性定量, 灵敏度高、抗干扰能力强、分析准确性好, 适用于复杂基质样品中农药残留检测。多数有机氯、有机磷及拟除虫菊酯类农药挥发性强, 加热容易气化, 用GC-MS/MS能取得较好的分析效果[18]。
本研究在充分调研目前普遍在用农药的基础上, 结合国家明文规定的禁限用农药清单、广东省农产品质量安全专项监测项目参数和农产品安全风险管控相关检测数据结果, 采用改进的QuEChERS法结合GC-MS/MS建立动物源性食品中58种农药残留的分析方法, 可通过一次简单的样品前处理, 实现58种农药的同时测定, 最大限度覆盖潜在风险隐患较大的农药, 旨在为动物源性食品中农药残留分析和市场安全监管提供技术支撑。
1 材料与方法
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1.1 材料与试剂
商场购买5种不同基质类型的动物源性食品为实验样品, 分别为猪肉、鸡肉、鱼肉、鸡蛋和牛奶, 将样品(牛奶除外)搅拌匀浆后, 装入干净的密封容器并贴好标签, 在-20 ℃冰箱中储存备用。
58种农药标准溶液(质量浓度均为1000 μg/mL)、环氧七氯A内标标准溶液(质量浓度为100 μg/mL)[农业农村部环境质量监督检验测试中心(天津)]; 乙腈、乙酸乙酯、正己烷(色谱纯, 德国Merck公司); 冰醋酸(色谱纯, 上海麦克林生化科技有限公司); 无水乙酸钠、氯化钠(优级纯, 国药集团化学试剂有限公司); 无水硫酸镁(优级纯)、柠檬酸钠、柠檬酸氢二钠(分析纯)(天津市光复科技发展有限公司); PSA(美国Agilent公司); 十八烷基硅烷键合硅胶(C18)(上海月旭科技公司); 0.22 μm有机微孔滤膜(上海安谱实验科技股份有限公司); 实验用水均为超纯水。
1.2 仪器与设备
Trace 1600-TSQ 9610气相色谱-串联质谱仪、TG-5SILMS气相色谱柱(30 m×0.25 mm, 0.25 μm)(美国Thermo Fisher Scientific公司); MS3基本型漩涡振荡器(德国IKA公司); METTLER TOLEDO PL602-L电子分析天平(精度0.0001 g, 瑞典梅特勒-多勒普公司); AS20500AT超声波清洗器(天津奥特赛恩斯公司); CL2001搅拌机(深圳艾美特电器有限公司); N-EVAP24全自动氮吹仪(美国Organomation公司); 3-30KS高速冷冻离心机(德国Sigma公司); Milli-Q超纯水机(美国Millipore公司)。
1.3 实验方法
1.3.1 标准工作溶液的配制
将58种农药标准溶液用乙酸乙酯转移定容至100 mL, 配制成58种农药混合标准储备溶液, 各组分的质量浓度均为10 mg/L。准确吸取一定量的混合标准储备溶液, 逐级用乙酸乙酯稀释成质量浓度为0.005、0.010、0.050、0.100、0.200、0.500 mg/L的标准工作溶液(现配现用)。空白基质溶液氮气吹干, 加入20 μL内标溶液(10 mg/L), 再分别加入1 mL上述标准工作溶液复溶, 过0.22 μm有机微孔滤膜配制成基质匹配标准工作溶液, 供GC-MS/MS仪测定。
1.3.2 样品前处理
称取5 g(精确至0.01 g)样品于50 mL具塞塑料离心管中, 加入1颗陶瓷振子和2 mL正己烷, 涡旋1 min, 再加入10 mL含1%冰醋酸的正己烷饱和乙腈溶液, 涡旋1 min, 超声提取10 min, 于-20 ℃冷冻15 min后, 加入1 g无水乙酸钠和4 g无水硫酸镁, 涡旋1 min, 于10000 r/min离心5 min。分取上清液5 mL, 加入15 mL具塞塑料离心管中(内含600 mg无水硫酸镁+100 mg PSA+100 mg C18), 涡旋1 min, 于10000 r/min离心5 min。取2 mL上清液转移至15 mL塑料离心管中, 于45 ℃水浴氮吹至近干, 加入20 μL内标溶液, 再加入1 mL乙酸乙酯复溶, 经0.22 μm有机微孔滤膜过滤后, 供GC-MS/MS仪测定。
1.4 仪器工作条件
1.4.1 色谱条件
色谱柱: TG-5SILMS气相色谱柱(30 m×0.25 mm, 0.25 μm); 载气: 高纯氦气, 纯度≥99.999%; 分流模式: 不分流进样; 进样口温度: 280 ℃; 流速: 1 mL/min; 进样量: 1.0 μL; 溶剂延迟3.5 min; 程序升温条件: 起始温度90 ℃, 保持1 min; 以40 ℃/min升至180 ℃, 保持2 min; 以10 ℃/min升至220 ℃保持1 min; 以30 ℃/min升至280 ℃保持7 min; 以40 ℃/min升至300 ℃, 保持3 min, 共23 min。
1.4.2 质谱条件
电离模式: 电子轰击离子化(electron impact, EI); 电离能量: 70 eV; 分析模式: 选择反应监测(selective reaction monitoring, SRM)模式; 碰撞气: 高纯氩气, 纯度≥99.999%; 离子源温度: 300 ℃; 传输线温度: 280 ℃。
1.5 数据处理
通过Chromeleon 7软件(美国Thermo Fisher Scientific公司)进行数据采集和预处理、生成标准曲线, 并进行内标法定量分析; 数据统计分析和柱状图、折线图、散点图用WPS office 2019软件完成。
2 结果与分析
收起
2.1 色谱条件的优化
由于大部分待测农药的分子极性较小, 所以本研究选用弱极性的TG-5SILMS气相色谱柱。对于多农药残留检测样品, 恒定柱温难以获得好的分离效果, 采取程序升温方法不但能改善分离效果, 还能缩短分析周期, 改善峰形, 提高检测灵敏度。通过优化色谱条件, 58种农药得到了有效分离, 能满足分析要求。
2.2 质谱条件的优化
SRM模式比单离子检测扫描(single ion monitoring, SIM)模式灵敏度更高、抗干扰能力更强、选择性更好, 更适合复杂基质中农药残留的测定[19]。为确保定性和定量的准确性, 本研究选择SRM模式, 首先对加入内标的农药标准溶液进行全扫描, 确定各农药及内标的出峰时间并选择质荷比大、信号强度高的一级碎片离子作为母离子, 然后在不同碰撞能量下对母离子进行二次电离, 选择信号最强的2~4个二级碎片离子作为子离子, 并对各离子对的碰撞能量进行优化, 选择干扰少、信号强度高的2个离子对分别作为定量离子对和定性离子对。进一步对离子源温度、传输线温度等条件进行优化, 得到最优质谱参数, 58种农药和内标的质谱参数见表1, 58种农药在优化条件下的SRM总离子流图见图1(图中58种农药序号与表1相同)。
2.3 前处理条件的优化
2.3.1 提取剂的选择
乙腈是农药残留检测常用的提取剂, 本研究所涉及的58种农药均在乙腈中有较好的溶解度。但是, 乙腈是极性溶剂, 与油脂不相溶, 不能将油脂中的待测农药提取出来[20]; 正己烷是非极性溶剂, 可以溶解油脂, 先加少量正己烷再加乙腈, 可以使乙腈更充分地与油脂接触, 提取油脂中的待测农药。有文献[21]报道, 在乙腈中加入正己烷不仅可提高非极性农药的提取效率, 而且有利于去除样品中的极性干扰成分, 降低基质的干扰。选取猪肉空白基质进行加标回收实验(n=3), 58种农药的加标水平均为0.1 mg/kg, 对比了先加2 mL正己烷, 再分别加10 mL乙腈、10 mL正己烷饱和乙腈、10 mL正己烷饱和乙腈(含1%冰醋酸)对提取效果的影响(见图2)。结果显示, 在只用乙腈作萃取溶剂时, 只有31种农药回收率在80%~110%, 原因可能是乙腈溶于正己烷会带走部分农药; 当用正己烷饱和乙腈作萃取溶剂进行提取时, 有45种农药回收率在80%~110%; 当用正己烷饱和乙腈(含1%冰醋酸)作提取剂时, 回收率在80%~110%的农药数量最高, 达到50种。因此, 选择正己烷饱和乙腈(含1%冰醋酸)作为提取剂。
2.3.2 提取方式的选择
实验对比了相同提取时间(5 min、10 min)下超声提取和振荡提取2种方式的提取效率。结果表明, 超声提取比振荡提取的效率高。进一步对超声提取时间进行优化, 发现超声10 min以后58种农药的平均回收率达到最大并趋于平稳, 因此, 实验选择超声10 min的提取方式。
2.3.3 盐的选择
样品在提取过程中, 溶液pH会影响某些对于酸碱度敏感的农药的回收率。有研究[22-23]报道, 在乙酸钠和1%(体积分数)冰醋酸组成的弱酸性缓冲盐体系中, 提取液处于pH约为5.5的平衡缓冲状态, 大部分农药的性质更稳定。本研究选择猪肉空白基质, 在0.1 mg/kg添加水平下进行加标回收实验(n=3), 比对了QuEChERS法的普通盐包(4 g无水硫酸镁+1 g氯化钠)、乙酸缓冲盐体系盐包(4 g无水硫酸镁+1 g无水乙酸钠)、柠檬酸缓冲盐体系盐包(4 g无水硫酸镁+1 g氯化钠+1 g柠檬酸钠+0.5 g柠檬酸氢二钠)对提取效果的影响(见图3, 图中58种农药序号与表2相同)。结果显示, 58种农药平均回收率大小依次为: 乙酸缓冲盐体系盐包(98.0%)>柠檬酸缓冲盐体系盐包(94.5%)>普通盐包(81.8%), 并且在使用乙酸缓冲盐体系盐包的条件下, 除了乙酰甲胺磷、氧乐果和甲霜灵以外, 其余农药的回收率均在80%~110%之间。因此, 实验选择乙酸缓冲盐体系盐包对提取液盐析。
2.3.4 冷冻时间的选择
无水硫酸镁是QuEChERS法常用的除水剂, 吸水放热时局部温度可达60 ℃以上, 会导致热不稳定的农药, 如甲胺磷、甲拌磷、氧乐果等回收率严重下降[24]。将提取液样品放入冰箱中冷冻后再加入无水硫酸镁, 可以解决发热量大的问题。实验比较了将提取液放入-20 ℃冰箱冷冻不同时间(5、10、15、20、25 min)对猪肉空白基质加标回收率(加标浓度0.1 mg/kg, n=3)的影响(见图4)。结果表明, 冷冻提取液能很好地解决由于发热量过大而导致农药回收率偏低的问题, 冷冻15 min以后回收率基本达到最高并趋于平稳。因此, 选择冷冻时间为15 min。
2.3.5 净化剂的选择
QuEChERS方法常用的净化剂有PSA、C18、石墨化碳黑(graphitized carbon black, GCB)、无水硫酸镁等。PSA能去除样本基质中的脂肪酸、糖等极性杂质, C18能吸附基质中部分非极性脂肪和脂溶性杂质, 无水硫酸镁能除去提取液中残留的水分, GCB能有效地去除色素和甾醇, 但同时也吸附具有平面结构的农药, 会导致农药回收率下降, 基质颜色不深时应尽量避免使用[25]。动物源性食品基质颜色一般较浅, 故选择PSA、C18和无水硫酸镁为净化剂。在固定加入600 mg无水硫酸镁条件下, 通过正交实验比较了C18添加量为50、100、150、200 mg, PSA添加量为50、100、150、200 mg对回收率的影响, 发现C18和PSA添加量均为100 mg时58种农药的平均回收率最高。因此, 实验最终选择600 mg无水硫酸镁、100 mg C18和100 mg PSA作为净化剂。
2.3.6 水浴温度和复溶液的选择
乙腈会加速气相色谱柱固定相流失, 降低柱效, 导致目标化合物峰拖尾和分裂, 因此需要将提取液中的乙腈水浴氮吹至近干, 然后进行溶剂置换。水浴温度不宜超过50 ℃, 否则热不稳定的农药回收率会严重下降, 综合考虑水浴氮吹效率和农药回收率, 将水浴温度设定为45 ℃。对于多农药残留分析, 一般选择中等极性的溶剂, 参考相关文献[26-27]和GB 23200.113—2018《食品安全国家标准 植物源性食品中208种农药及其代谢物残留量的测定 气相色谱-质谱联用法》, 实验选择乙酸乙酯作为复溶液。
2.4 基质效应
对溶剂标样和基质空白标样分别进样分析, 测得峰面积分别为A和B, 基质效应(matrix effect, ME)=(B/A-1)× 100%, ME>0时为基质增强效应, ME<0时为基质抑制效应。|ME|≤20%、20%<|ME|≤50%、|ME|>50%分别表示弱ME(可忽略)、中等ME、较强ME[28-29]。本研究中, 猪肉、鸡肉、鱼肉、鸡蛋和牛奶中均有不少农药存在中等或较强的ME(见图5, 图中58种农药序号与表2相同)。为尽可能消除ME的影响, 保证检测结果的准确性, 本方法采用空白基质匹配标准曲线内标法定量。
2.5 方法学验证
2.5.1 方法选择性
本方法通过保留时间及所选特征离子对进行定性和定量, 对猪肉、鸡肉、鱼肉、鸡蛋和牛奶空白加标样品进行考察, 发现各农药所选择的定性与定量离子在保留时间附近均无明显干扰, 表明方法具有较好的选择性。
2.5.2 线性关系、检出限与定量限
选择猪肉空白基质, 按方法“1.3”逐级稀释成各农药组分质量浓度分别为0.005、0.010、0.050、0.100、0.200、0.500 mg/L而建立基质匹配工作曲线, 以农药质量浓度(X, mg/L)为横坐标, 农药定量离子峰面积和内标定量离子峰面积的比值(Y)为纵坐标, 绘制标准曲线(见表2)。结果显示, 在0.005~0.500 mg/L范围内, 58种农药均呈现良好的线性关系, 相关系数(r2)均大于0.9945。以定量离子响应的3倍信噪比(S/N=3)确定检出限, 以定量离子响应的10倍信噪比(S/N=10)确定定量限, 得到58种农药的检出限为0.001~0.005 mg/kg, 定量限为0.002~0.015 mg/kg, 本方法可满足相关限量分析的需求。
2.5.3 回收率与相对标准偏差
选择猪肉、鸡肉、鱼肉、鸡蛋和牛奶空白基质, 分别添加0.02、0.05、0.20 mg/kg 3个浓度水平的混合标准溶液, 按本研究的方法进行提取和净化, 每个添加水平重复测定4次, 在0.02、0.05、0.20 mg/kg 3个添加水平下, 各种农药在猪肉、鸡肉、鱼肉、鸡蛋和牛奶中的回收率(见表3)分别为72.6%~117.4%、71.8%~115.2%、82.5%~106.8%, 相对标准偏差分别为0.8%~8.7%、1.2%~5.8%、0.7%~7.0%。方法的准确度和精密度符合GB/T 27404—2008《实验室质量控制规范 食品理化检测》的规定, 满足农药残留分析的要求。
2.5.4 实际样品测定
在超市和农贸市场抽取5份猪肉样品和3份鸡肉样品, 按照本方法进行测定, 样品均未检出农药。
3 结论
收起
本研究通过改进QuEChERS前处理方法, 建立了GC-MS/MS测定动物源性食品中58种农药残留的检测方法。该方法简单快速, 选择性好, 检出限低, 准确度高, 适用于动物源性食品中农药残留的检测。但是, 动物源性食品种类繁多, 本研究所选取的5种样品无法覆盖全部动物源性食品, 仍需对动物内脏、甲壳动物、蜂蜜、燕窝等其他动物源性食品进行实验比对, 进一步验证该方法的适用性。另外, 内标法包括内标前置法(样品前处理前加入内标)和内标后置法(样品前处理后加入内标)[30], 本研究采用的是内标后置法, 可以消除仪器不稳定带来的误差, 却无法补偿样品前处理过程中提取、转移、氮吹等环节待测农药组分的损失。后续研究中可以对内标前置法进行方法学验证, 并对提取条件和净化条件不断改进, 以期为动物源性食品中农药残留检测和风险评估提供更优的技术方法。
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2025年第16卷第5期
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doi: 10.19812/j.cnki.jfsq11-5956/ts.20240823004
  • 接收时间：2024-08-23
  • 首发时间：2025-07-19
  • 出版时间：2025-03-15
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  • 收稿日期：2024-08-23
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    深圳市农产品质量安全检验检测中心, 深圳 518055

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* 杨凯(1987—), 男, 硕士, 农艺师, 主要研究方向为农产品质量安全监测。E-mail:
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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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