Article(id=1240722568303398955, tenantId=1146029695717560320, journalId=1227665162245664772, issueId=1240722566957027366, articleNumber=null, orderNo=null, doi=10.20043/j.cnki.MPM.202505059, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1746374400000, receivedDateStr=2025-05-05, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1773740911793, onlineDateStr=2026-03-17, pubDate=1760025600000, pubDateStr=2025-10-10, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1773740911793, onlineIssueDateStr=2026-03-17, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1773740911793, creator=13701087609, updateTime=1773740911793, updator=13701087609, issue=Issue{id=1240722566957027366, tenantId=1146029695717560320, journalId=1227665162245664772, year='2025', volume='52', issue='19', pageStart='3457', pageEnd='3648', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=1, specialIssue=0, createTime=1773740911472, creator=13701087609, updateTime=1773740981732, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1240722861736906836, tenantId=1146029695717560320, journalId=1227665162245664772, issueId=1240722566957027366, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1240722861736906837, tenantId=1146029695717560320, journalId=1227665162245664772, issueId=1240722566957027366, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=3620, endPage=3626, ext={EN=ArticleExt(id=1240722568710246445, articleId=1240722568303398955, tenantId=1146029695717560320, journalId=1227665162245664772, language=EN, title=Determination of 15 N-nitrosamines in bacon by QuEChERS purification and gas chromatography-tandem mass spectrometry, columnId=1228016572065837304, journalTitle=Modern Preventive Medicine, columnName=Experimental Technology and Applications, runingTitle=null, highlight=null, articleAbstract=
Objective To establish a method for the rapid detection of 15 N-nitrosamines in bacon by enhanced matrix removal dispersive solid phase extraction combined with gas chromatography-tandem mass spectrometry (GC-MS/MS). Methods The samples were extracted with acetonitrile oscillation, frozen for 30 minutes, and then centrifuged at low temperature. The extract was further purified using an enhanced lipid removal purification tube (QuEChERS EMR-lipid) and an EMR-lipid stripping tube. The N-nitrosamines were separated on a polar capillary column, detected in the multiple reaction monitoring (MRM) mode and quantified by the matrix-matched external standard method. Results The linear correlation coefficients of the method were greater than 0.990 in the range of 0.2-40.0 μg/L, with the detection and quantification limits of 0.03-0.30 and 0.1-1.0 μg/kg, respectively. The recoveries were 64.1%-106.1% at three spiked levels (2.0, 5.0, 10.0 μg/kg),with the relative standard deviations (RSDs) ranging from 3.48% to 14.55%. Conclusion The method does not require activation, equilibration, or elution steps, consumes less solvent, is simple and rapid, and is suitable for the rapid detection of 15 N-nitrosamines in bacon.
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目的 建立腊肉中15种N-亚硝胺类化合物的增强型基质去除分散固相萃取结合气相色谱串联质谱(GC-MS/MS)快速测定方法。方法 样品经乙腈振荡提取,冷冻30 min后低温离心,提取液经增强型脂质去除净化管(QuEChERS EMR-Lipid)和EMR-Lipid反萃管进一步净化,目标物经极性毛细管柱分离后以多反应监测模式(MRM)检测和基质匹配外标法定量。结果 在0.2~40.0 μg/L范围内线性相关系数均大于0.990,方法检出限及定量限分别为0.03~0.30 μg/kg和0. 1~1.0 μg/kg。三个水平(2.0、5.0和10.0 μg/kg)的加标回收率范围为64.1%~106.1%,相对标准偏差为3.48%~14.55%。结论 本法无需活化、平衡、洗脱步骤,消耗溶剂较少,操作简单,适用于腊肉中N-亚硝胺类化合物的快速检测。
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本刊刊出的所有文章不代表中华预防医学会和本刊编委会的观点,除非特别声明。, copyrightOwner=中华预防医学会和四川大学华西公共卫生学院, extLink=null, articleAbsUrl=null, sourceXml=DFLx+L8O4djPLlnM1yTDCw==, magXml=ZrN1RgCXIZX05lEnKvsNIA==, pdfUrl=null, pdf=8AIXhCTd4qcMINChIwZ8pQ==, pdfFileSize=1189196, pdfExtLink=null, richHtmlUrl=null, mobilePdfUrl=null, reviewReport=null, pdfFirstPage=null, abstractGraph=2c3X55nrGd/zm1Zs/I0aQw==, abstractGraphContent=null, abstractVideo=null, citation=null, cebUrl=null, magXmlContent=BqubUzorI05CwYtafvXWsg==, mapNumber=null, authorCompany=null, fund=null, authors=
张权(1988—),男,硕士,主管技师,研究方向:食品及环境中污染物分析
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The recovery comparisom of different extraction solvents, figureFileSmall=YxVKIWy3UpIgzNxRZnqllQ==, figureFileBig=fLL6jFiN9wglMbnZT9gLJg==, tableContent=null), ArticleFig(id=1240933512971342196, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1240722568303398955, language=CN, label=图1, caption=
不同提取剂的回收率比较, figureFileSmall=YxVKIWy3UpIgzNxRZnqllQ==, figureFileBig=fLL6jFiN9wglMbnZT9gLJg==, tableContent=null), ArticleFig(id=1240933513067811192, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1240722568303398955, language=EN, label=Figure 2, caption=
The full scan spectrogram of the sample solutions by different purification methods, figureFileSmall=oN7S/a5oOWQzmIDx1Dw2Rg==, figureFileBig=9AL8Wvul2tCmpFnFcaY3UA==, tableContent=null), ArticleFig(id=1240933513151697275, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1240722568303398955, language=CN, label=图2, caption=
不同净化方式的样品液全扫谱图注:图A为Dima QuEChERS;图B为Agela QuEChERS;图C为EMR-Lipid dSPE;图D为LPAS-SPE;图E为HLB-SPE;图F为Captiva EMR-Lipid HF-SPE;图G为CNW QuEChERS。
, figureFileSmall=oN7S/a5oOWQzmIDx1Dw2Rg==, figureFileBig=9AL8Wvul2tCmpFnFcaY3UA==, tableContent=null), ArticleFig(id=1240933513235583360, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1240722568303398955, language=EN, label=Figure 3, caption=
Total ion chromatogram of a spiked bacon sample, figureFileSmall=1Ts61Qt+srLdlKT0gD/dWA==, figureFileBig=d/iCla1FbozmIiwszm3Igw==, tableContent=null), ArticleFig(id=1240933513319469444, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1240722568303398955, language=CN, label=图3, caption=
腊肉加标样品的总离子流色谱图, figureFileSmall=1Ts61Qt+srLdlKT0gD/dWA==, figureFileBig=d/iCla1FbozmIiwszm3Igw==, tableContent=null), ArticleFig(id=1240933513390772615, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1240722568303398955, language=EN, label=Table 1, caption=
The mass spectrometric parameters of the method
, figureFileSmall=null, figureFileBig=null, tableContent=
| 序号 | 化合物 | 化学式 | CAS | 保留时间(min) | 离子对(m/z) | 碰撞能量(eV) |
|---|
| 1 | N-亚硝基二甲胺(NDMA) | C2H6N2O | 62-75-9 | 5.81 | 74.0>44.0*,74.0>42.1 | 3, 19 |
| 2 | N-亚硝基甲乙胺(NMEA) | C3H8N2O | 10595-95-6 | 6.40 | 88.0>71.1*,88.0>42.0 | 2, 17 |
| 3 | N-亚硝胺二乙胺(NDEA) | C4H10N2O | 55-18-5 | 6.75 | 102.0>85.0*,102.0>56.0 | 2, 15 |
| 4 | N-亚硝胺吡咯啶(NPYR) | C4H8N2O | 930-55-2 | 11.69 | 100.0>55.1*,100.0>43.1 | 5, 9 |
| 5 | N-亚硝胺甲基苯胺(NMPhA) | C7H5N2O | 614-00-6 | 10.94 | 107.0>106.0*,107.0>77.0 | 10, 15 |
| 6 | N-亚硝胺吗啉(NMorPh) | C4H8N2O2 | 59-89-2 | 12.66 | 116.0>56.0*,116.2>86.1 | 11, 5 |
| 7 | N-亚硝胺二丙胺(NDPA) | C6H14N2O | 621-64-7 | 8.43 | 130.2>43.0*,130.2>113.1 | 9, 7 |
| 8 | N-亚硝胺哌啶(NPIP) | C5H10N2O | 100-75-4 | 11.16 | 114.0>84.0*,114.0>41.0 | 5, 13 |
| 9 | N-亚硝胺乙基苯胺(NEPhA) | C8H10N2O | 612-64-6 | 10.99 | 121.0>106.0*,121.0>77.0 | 5, 20 |
1 0 | N-亚硝基二正丁胺(NDBA) | C8H18N2O | 924-16-3 | 10.78 | 116.0>99.0*,116.0>74.1 | 2, 8 |
| 11 | N-亚硝胺二苯胺(NDPhA) | C12H10N2O | 86-30-6 | 18.91 | 169.0>168.1*,169.0>167.1 | 17, 30 |
| 12 | N-亚硝胺二苄胺(NDBzA) | C14H14N2O | 5336-53-8 | 21.95 | 226.0>91.0*,91.0>65.0 | 5, 5 |
| 13 | N-亚硝胺乙基异丙基胺(NEIPA) | C5H12N2O | 16339-04-1 | 7.17 | 116.0>99.0*,116.0>44.0 | 5, 15 |
| 14 | N-亚硝胺二异丙胺(NDiPA) | C6H14N2O | 601-77-4 | 7.49 | 130.0>88.0*,130.0>42.0 | 5, 10 |
| 15 | N-亚硝胺二异丁胺(NDIBA) | C8H18N2O | 997-95-5 | 8.69 | 84.0>57.0*,115.0>84.0 | 5, 3 |
), ArticleFig(id=1240933513470464393, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1240722568303398955, language=CN, label=表1, caption=
方法的质谱参数
, figureFileSmall=null, figureFileBig=null, tableContent=
| 序号 | 化合物 | 化学式 | CAS | 保留时间(min) | 离子对(m/z) | 碰撞能量(eV) |
|---|
| 1 | N-亚硝基二甲胺(NDMA) | C2H6N2O | 62-75-9 | 5.81 | 74.0>44.0*,74.0>42.1 | 3, 19 |
| 2 | N-亚硝基甲乙胺(NMEA) | C3H8N2O | 10595-95-6 | 6.40 | 88.0>71.1*,88.0>42.0 | 2, 17 |
| 3 | N-亚硝胺二乙胺(NDEA) | C4H10N2O | 55-18-5 | 6.75 | 102.0>85.0*,102.0>56.0 | 2, 15 |
| 4 | N-亚硝胺吡咯啶(NPYR) | C4H8N2O | 930-55-2 | 11.69 | 100.0>55.1*,100.0>43.1 | 5, 9 |
| 5 | N-亚硝胺甲基苯胺(NMPhA) | C7H5N2O | 614-00-6 | 10.94 | 107.0>106.0*,107.0>77.0 | 10, 15 |
| 6 | N-亚硝胺吗啉(NMorPh) | C4H8N2O2 | 59-89-2 | 12.66 | 116.0>56.0*,116.2>86.1 | 11, 5 |
| 7 | N-亚硝胺二丙胺(NDPA) | C6H14N2O | 621-64-7 | 8.43 | 130.2>43.0*,130.2>113.1 | 9, 7 |
| 8 | N-亚硝胺哌啶(NPIP) | C5H10N2O | 100-75-4 | 11.16 | 114.0>84.0*,114.0>41.0 | 5, 13 |
| 9 | N-亚硝胺乙基苯胺(NEPhA) | C8H10N2O | 612-64-6 | 10.99 | 121.0>106.0*,121.0>77.0 | 5, 20 |
1 0 | N-亚硝基二正丁胺(NDBA) | C8H18N2O | 924-16-3 | 10.78 | 116.0>99.0*,116.0>74.1 | 2, 8 |
| 11 | N-亚硝胺二苯胺(NDPhA) | C12H10N2O | 86-30-6 | 18.91 | 169.0>168.1*,169.0>167.1 | 17, 30 |
| 12 | N-亚硝胺二苄胺(NDBzA) | C14H14N2O | 5336-53-8 | 21.95 | 226.0>91.0*,91.0>65.0 | 5, 5 |
| 13 | N-亚硝胺乙基异丙基胺(NEIPA) | C5H12N2O | 16339-04-1 | 7.17 | 116.0>99.0*,116.0>44.0 | 5, 15 |
| 14 | N-亚硝胺二异丙胺(NDiPA) | C6H14N2O | 601-77-4 | 7.49 | 130.0>88.0*,130.0>42.0 | 5, 10 |
| 15 | N-亚硝胺二异丁胺(NDIBA) | C8H18N2O | 997-95-5 | 8.69 | 84.0>57.0*,115.0>84.0 | 5, 3 |
), ArticleFig(id=1240933513541767566, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1240722568303398955, language=EN, label=Table 2, caption=
The performance parameters of the method(n=6)
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| 被测化合物 | 线性范围 (μg/L) | 回归方程 | 相关系数 (r2) | 检出限 (μg/kg) | 定量限 (μg/kg) | 2.00 μg/kg | 5.00 μg/kg | 10.0 μg/kg |
|---|
回收率 (%) | RSD (%) | 回收率 (%) | RSD (%) | 回收率 (%) | RSD (%) |
|---|
| NDMA | 0.2~40.0 | Y=3.311×103X+7.830×105 | 0.996 4 | 0.15 | 0.5 | 87.2 | 9.36 | 94.4 | 13.86 | 87.9 | 10.71 |
| NMEA | 0.2~40.0 | Y=3.027×103X-4.002×103 | 0.998 8 | 0.15 | 0.5 | 93.4 | 7.55 | 95.2 | 6.02 | 83.3 | 8.92 |
| NDEA | 0.2~40.0 | Y=2.313×103X-1.195×103 | 0.999 2 | 0.15 | 0.5 | 85.3 | 9.48 | 84.5 | 11.37 | 76.7 | 10.25 |
| NPYR | 0.2~40.0 | Y=1.889×103X-2.395×103 | 0.998 4 | 0.15 | 0.5 | 84.5 | 14.33 | 88.1 | 14.38 | 81.5 | 3.48 |
| NMPhA | 0.2~40.0 | Y=1.193×104X-1.990×104 | 0.996 8 | 0.03 | 0.1 | 99.1 | 7.79 | 85.4 | 3.57 | 86.3 | 14.28 |
| NMorPh | 0.2~40.0 | Y=9.347×102X-6.099×103 | 0.999 2 | 0.15 | 0.5 | 84.3 | 10.30 | 94.6 | 4.69 | 81.5 | 9.39 |
| NDPA | 0.2~40.0 | Y=5.091×102X-5.373×102 | 0.999 4 | 0.30 | 1.0 | 88.8 | 13.56 | 93.1 | 12.05 | 83.5 | 7.88 |
| NPIP | 0.2~40.0 | Y=1.876×103X-4.781×103 | 0.997 7 | 0.15 | 0.5 | 96.1 | 12.58 | 95.7 | 11.39 | 86.1 | 10.54 |
| NEPhA | 0.2~40.0 | Y=1.140×104X+4.497×103 | 0.999 0 | 0.03 | 0.1 | 77.1 | 8.67 | 87.9 | 8.54 | 83.8 | 4.77 |
| NDBA | 0.2~40.0 | Y=2.090×103X-8.528×102 | 0.998 6 | 0.15 | 0.5 | 85.6 | 10.36 | 93.0 | 9.36 | 82.8 | 10.81 |
| NDPhA | 0.2~40.0 | Y=1.088×105X+4.258×105 | 0.999 6 | 0.03 | 0.1 | 106.1 | 5.36 | 101.1 | 7.58 | 86.8 | 8.36 |
| NDBzA | 0.2~40.0 | Y=1.038×103X-9.962×102 | 0.999 0 | 0.15 | 0.5 | 91.5 | 7.48 | 80.9 | 8.95 | 80.7 | 12.38 |
| NEIPA | 0.2~40.0 | Y=2.772×103X-1.152×103 | 0.998 8 | 0.15 | 0.5 | 64.1 | 12.39 | 73.7 | 6.52 | 81.8 | 14.55 |
| NDiPA | 0.2~40.0 | Y=1.213×103X-6.851×102 | 0.997 8 | 0.15 | 0.5 | 78.4 | 10.36 | 99.0 | 7.36 | 87.2 | 7.96 |
| NDIBA | 0.2~40.0 | Y=5.972×102X-2.420×101 | 0.996 9 | 0.10 | 0.3 | 82.3 | 14.21 | 83.8 | 11.3 | 75.0 | 4.56 |
), ArticleFig(id=1240933513646625168, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1240722568303398955, language=CN, label=表2, caption=
方法的性能参数(n=6)
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| 被测化合物 | 线性范围 (μg/L) | 回归方程 | 相关系数 (r2) | 检出限 (μg/kg) | 定量限 (μg/kg) | 2.00 μg/kg | 5.00 μg/kg | 10.0 μg/kg |
|---|
回收率 (%) | RSD (%) | 回收率 (%) | RSD (%) | 回收率 (%) | RSD (%) |
|---|
| NDMA | 0.2~40.0 | Y=3.311×103X+7.830×105 | 0.996 4 | 0.15 | 0.5 | 87.2 | 9.36 | 94.4 | 13.86 | 87.9 | 10.71 |
| NMEA | 0.2~40.0 | Y=3.027×103X-4.002×103 | 0.998 8 | 0.15 | 0.5 | 93.4 | 7.55 | 95.2 | 6.02 | 83.3 | 8.92 |
| NDEA | 0.2~40.0 | Y=2.313×103X-1.195×103 | 0.999 2 | 0.15 | 0.5 | 85.3 | 9.48 | 84.5 | 11.37 | 76.7 | 10.25 |
| NPYR | 0.2~40.0 | Y=1.889×103X-2.395×103 | 0.998 4 | 0.15 | 0.5 | 84.5 | 14.33 | 88.1 | 14.38 | 81.5 | 3.48 |
| NMPhA | 0.2~40.0 | Y=1.193×104X-1.990×104 | 0.996 8 | 0.03 | 0.1 | 99.1 | 7.79 | 85.4 | 3.57 | 86.3 | 14.28 |
| NMorPh | 0.2~40.0 | Y=9.347×102X-6.099×103 | 0.999 2 | 0.15 | 0.5 | 84.3 | 10.30 | 94.6 | 4.69 | 81.5 | 9.39 |
| NDPA | 0.2~40.0 | Y=5.091×102X-5.373×102 | 0.999 4 | 0.30 | 1.0 | 88.8 | 13.56 | 93.1 | 12.05 | 83.5 | 7.88 |
| NPIP | 0.2~40.0 | Y=1.876×103X-4.781×103 | 0.997 7 | 0.15 | 0.5 | 96.1 | 12.58 | 95.7 | 11.39 | 86.1 | 10.54 |
| NEPhA | 0.2~40.0 | Y=1.140×104X+4.497×103 | 0.999 0 | 0.03 | 0.1 | 77.1 | 8.67 | 87.9 | 8.54 | 83.8 | 4.77 |
| NDBA | 0.2~40.0 | Y=2.090×103X-8.528×102 | 0.998 6 | 0.15 | 0.5 | 85.6 | 10.36 | 93.0 | 9.36 | 82.8 | 10.81 |
| NDPhA | 0.2~40.0 | Y=1.088×105X+4.258×105 | 0.999 6 | 0.03 | 0.1 | 106.1 | 5.36 | 101.1 | 7.58 | 86.8 | 8.36 |
| NDBzA | 0.2~40.0 | Y=1.038×103X-9.962×102 | 0.999 0 | 0.15 | 0.5 | 91.5 | 7.48 | 80.9 | 8.95 | 80.7 | 12.38 |
| NEIPA | 0.2~40.0 | Y=2.772×103X-1.152×103 | 0.998 8 | 0.15 | 0.5 | 64.1 | 12.39 | 73.7 | 6.52 | 81.8 | 14.55 |
| NDiPA | 0.2~40.0 | Y=1.213×103X-6.851×102 | 0.997 8 | 0.15 | 0.5 | 78.4 | 10.36 | 99.0 | 7.36 | 87.2 | 7.96 |
| NDIBA | 0.2~40.0 | Y=5.972×102X-2.420×101 | 0.996 9 | 0.10 | 0.3 | 82.3 | 14.21 | 83.8 | 11.3 | 75.0 | 4.56 |
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