主题：【资料搜集】霜霉威检测方法

Determination of propamocarb in vegetables using polymer-based high-performance liquid chromatography coupled with electrospray mass spectrometry
Maurice Hiemstra,and André de Kok
Journal of Chromatography A;Volume 972, Issue 2, 4 October 2002, Pages 231-239
Abstract:
A method for the determination of propamocarb in vegetables with liquid chromatography–electrospray ionisation mass spectrometry ($$lc–ESI-MS) was developed. The performance of a polymer-based analytical $$lc column for the separation was investigated. Residues of propamocarb were extracted from the matrix with methanol. Subsequently, the extract was directly injected into the $$lc–MS system, without any additional concentration or cleanup procedures. Separation of propamocarb from the matrix components was achieved on a polymethacrylate-based analytical column. Propamocarb was concurrently detected with electrospray ionisation mass spectrometry in the selected ion monitoring mode and two-stage full scan MS application. Quantitation was done with matrix-matched calibration standards of propamocarb. Unambiguous confirmation was achieved by comparison of the full scan product ion mass spectrum of the chromatographic peak in the sample with the spectrum of a standard solution of propamocarb at the same retention time. The analytical performance of the method was validated for five relevant matrices, spiking propamocarb at fortification levels from 0.05 to 15.0 mg kg−1. This covers the range of maximum residue limits in agricultural commodities, stated in the Dutch national legislation. The mean recovery of propamocarb was better than 90% with a precision of less than 10% in both scanning applications. As could be concluded from the calibration curve and matrix background levels, observed in blank control samples, the estimated limit of detection was 25 μg kg−1 for the two-stage full scan MS application. The method has been applied in a survey of 285 samples of lettuce, radish, leek, and cabbage for the presence of residues of propamocarb. In 50% of the samples analysed, a residue of propamocarb was detected.

  http://www.sciencedirect.com/science?_ob=ArticleURL&_udi=B6TG8-46P1PRX-B&_user=10&_rdoc=1&_fmt=&_orig=search&_sort=d&view=c&_acct=C000050221&_version=1&_urlVersion=0&_userid=10&md5=fc5a5a9af3df12563e6c9d4637295e7f

Determination of residues of propamocarb in wine by liquid chromatography-electrospray mass spectrometry with direct injection
J. C. Taylor;  S. J. Hird;  M. D. Sykes; J. R. Startin
Food Additives & Contaminants: Part A, Volume 21, Issue 6 June 2004 , pages 572 - 577

Abstract
A simple, sensitive and reliable liquid chromatography-mass spectrometry method with direct injection of diluted samples is reported for the determination of propamocarb residues in wine. Red and white wines were diluted 40- and 20-fold, respectively, using water. Liquid chromatography was performed with a mobile-phase gradient and detection was by electrospray mass spectrometry in a positive ionization mode. Propamocarb was detected as the protonated molecular species at m/z 189. Using matrix-matched calibrant solutions, a calibrated range equivalent to 0.05-2.0 mg kg^-1 in red and white wines and limits of detection of 0.025 mg kg^-1 for white wine and of 0.05 mg kg^-1 for red wine (0.00125 μg ml^-1 of sample solution injected) were readily achievable. Recovery of propamocarb hydrochloride from wine spiked before dilution was in the range 91-115%. The chromatograms were free of isobaric interferences. In a small wine survey (72 samples), no residues of propamocarb were detected above 0.1 mg kg^-1.

    http://www.informaworld.com/smpp/content~content=a713599761~db=all

Gas chromatographic determination of propamocarb in agricultural commodities
NAGAYAMA T. et al.;
Journal of AOAC International; 1996, vol. 79, no3, pp. 769-772 (5 ref.)

Abstract:
A simple and efficient gas chromatographic (gc) method is described for quantitative determination of propamocarb in agricultural commodities. Propamocarb is extracted into acetone-water (or acidified solvent for dry products) and then cleaned up by extraction with diethyl ether. The analyte is extracted from the aqueous fraction under basic conditions with diethyl ether and then analyzed by gc with nitrogen-phosphorus detection. The minimum detection limit is 0.01 μg/g in original samples (signal-to-noise ratio > 5). Recovery of propamocarb spiked at 0.1 μg/g into various samples is >75%, except for lettuce (41%).
  http://cat.inist.fr/?aModele=afficheN&cpsidt=3091250

原文由 我在故我思(hotdoglet) 发表:
Gas chromatographic determination of propamocarb in agricultural commodities
NAGAYAMA T. et al.;
Journal of AOAC International; 1996, vol. 79, no3, pp. 769-772 (5 ref.)

Abstract:
A simple and efficient gas chromatographic (gc) method is described for quantitative determination of propamocarb in agricultural commodities. Propamocarb is extracted into acetone-water (or acidified solvent for dry products) and then cleaned up by extraction with diethyl ether. The analyte is extracted from the aqueous fraction under basic conditions with diethyl ether and then analyzed by gc with nitrogen-phosphorus detection. The minimum detection limit is 0.01 μg/g in original samples (signal-to-noise ratio > 5). Recovery of propamocarb spiked at 0.1 μg/g into various samples is >75%, except for lettuce (41%).
  http://cat.inist.fr/?aModele=afficheN&cpsidt=3091250

楼主，能否提供一下这篇文献，谢谢

原文由 核桃(pjs123) 发表:
霜霉威检测方法
1．分析目标化合物
霜霉威、霜霉威盐酸盐
2．仪器设备
带碱热离子检测器或高灵敏度氮磷检测器的气相色谱仪和气相色谱—质谱
仪。
3．试剂
使用附录2所列试剂。
4．标准品
霜霉威：含霜霉威99％以上，熔点为45℃～55℃。
5．试验溶液的制备
谷类：将样品粉碎，通过420μm的标准网筛后，称取其20.0g，加入30mL 1mol／L盐酸，放置2小时。
水果和蔬菜：准确称取约1 kg样品，必要时定量加入适量水，搅碎混合均匀后，称取相当于20.0g样品的量。
加入80 mL丙酮：水（7：3）混合溶液（谷类为50mL），搅拌5分钟后，用涂布1cm厚硅藻土的滤纸抽滤于磨口减压浓缩器中。取出滤纸上的残留物，加入50mL丙酮：水（7：3）混合溶液，搅拌5分钟后，按上述同样操作，合并滤液于减压浓缩器中，40℃以下浓缩至约40mL。将其移入预先注入50mL乙醚和5g氯化钠的200mL分液漏斗中，振摇混合1分钟后，静置，弃去乙醚层。水层中加入50mL乙醚，按上述同样操作，水层移入200mL分液漏斗中。水层中加入5g无水碳酸钠（谷类为8g）和50mL乙醚，用振荡器激烈振荡5分钟后，静置，乙醚层移入200mL三角瓶中。水层中加入50mL乙醚，按上述同样操作，重复2次，合并乙醚层于上述三角瓶中。加入适量无水硫酸钠，不时振摇、混合，放置15分钟后，滤入磨口减压浓缩器中。再用10ml乙醚洗涤三角瓶，以此洗液洗涤滤纸上的残留物，重复操作两次。合并两洗液于减压浓缩器中，40℃以下浓缩至约1mL，室温下通空气进一步干燥。残留物中加入乙酸乙酯溶解，
准确至1mL，此为试验溶液。
6．操作方法
a 定性试验
按下列操作条件进行试验，试验结果应与标准品的一致。
操作条件
柱：内径0.25mm、长30m的石英毛细管，涂布0.25μm厚气相色谱用14％氰丙基苯基—甲基硅酮，老化。
柱温：在60℃保持1分钟，此后每分钟升温10℃。到达160℃后保持2分钟，再每分钟升温4℃。到达180℃后每分钟升温20℃，到达260℃后保持5分钟。
进样器温度：250℃
进样方式：不分流
检测器温度：250℃
气体流量：以氦气作载气。调节流速使霜霉威约14分钟30秒流出。调节空气和氢气的流量至适当条件。
b 定量试验
根据与a 定性试验相同试验条件所得的试验结果，峰高法或峰面积法定量。
c 确证试验
按照与a 定性试验相同的试验条件，用气相色谱—质谱仪测定，试验结果应与标准品的一致。此外，必要时用峰高法或峰面积法进行定量。
7．定量限
0.01 mg/kg
8．注意事项
霜霉威的分析值包括霜霉威和霜霉威盐酸盐。
9．参考文献
无

很强悍!回收率什么水平?

原文由 MMYG(jl070869) 发表:

原文由 核桃(pjs123) 发表:
霜霉威检测方法
1．分析目标化合物
霜霉威、霜霉威盐酸盐
2．仪器设备
带碱热离子检测器或高灵敏度氮磷检测器的气相色谱仪和气相色谱—质谱仪。
3．试剂
使用附录2所列试剂。
4．标准品
霜霉威：含霜霉威99％以上，熔点为45℃～55℃。
5．试验溶液的制备
谷类：将样品粉碎，通过420μm的标准网筛后，称取其20.0g，加入30mL 1mol／L盐酸，放置2小时。
水果和蔬菜：准确称取约1 kg样品，必要时定量加入适量水，搅碎混合均匀后，称取相当于20.0g样品的量。
加入80 mL丙酮：水（7：3）混合溶液（谷类为50mL），搅拌5分钟后，用涂布1cm厚硅藻土的滤纸抽滤于磨口减压浓缩器中。取出滤纸上的残留物，加入50mL丙酮：水（7：3）混合溶液，搅拌5分钟后，按上述同样操作，合并滤液于减压浓缩器中，40℃以下浓缩至约40mL。将其移入预先注入50mL乙醚和5g氯化钠的200mL分液漏斗中，振摇混合1分钟后，静置，弃去乙醚层。水层中加入50mL乙醚，按上述同样操作，水层移入200mL分液漏斗中。水层中加入5g无水碳酸钠（谷类为8g）和50mL乙醚，用振荡器激烈振荡5分钟后，静置，乙醚层移入200mL三角瓶中。水层中加入50mL乙醚，按上述同样操作，重复2次，合并乙醚层于上述三角瓶中。加入适量无水硫酸钠，不时振摇、混合，放置15分钟后，滤入磨口减压浓缩器中。再用10ml乙醚洗涤三角瓶，以此洗液洗涤滤纸上的残留物，重复操作两次。合并两洗液于减压浓缩器中，40℃以下浓缩至约1mL，室温下通空气进一步干燥。残留物中加入乙酸乙酯溶解，
准确至1mL，此为试验溶液。
6．操作方法
a 定性试验
按下列操作条件进行试验，试验结果应与标准品的一致。
操作条件
柱：内径0.25mm、长30m的石英毛细管，涂布0.25μm厚气相色谱用14％氰丙基苯基—甲基硅酮，老化。
柱温：在60℃保持1分钟，此后每分钟升温10℃。到达160℃后保持2分钟，再每分钟升温4℃。到达180℃后每分钟升温20℃，到达260℃后保持5分钟。
进样器温度：250℃
进样方式：不分流
检测器温度：250℃
气体流量：以氦气作载气。调节流速使霜霉威约14分钟30秒流出。调节空气和氢气的流量至适当条件。
b 定量试验
根据与a 定性试验相同试验条件所得的试验结果，峰高法或峰面积法定量。
c 确证试验
按照与a 定性试验相同的试验条件，用气相色谱—质谱仪测定，试验结果应
与标准品的一致。此外，必要时用峰高法或峰面积法进行定量。
7．定量限
0.01 mg/kg
8．注意事项
霜霉威的分析值包括霜霉威和霜霉威盐酸盐。
9．参考文献
无

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这个方法可能是日本一律基准方法公布前的公定法之类的方法，格式很像，按照一律基准方法中的一齐分析法做，回收率不好。