食品中非食用物质的快速筛查及食品组学
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• 在一个系统上自动完成两种不同（互补）技术的方法筛选
一个样品序列可在SFC 与 LC之间相互切换 LC 与 SFC之间无需平衡 无需仪器变化即可直接进行SFC 与 LC 的结果比较 Simply switch the valve
• Save significant cost and laboratory space
November 7, 2015 7
牛油果中脂肪含量达20%！
Pesticides in Avocado
牛油果中的农残
November 7, 2015 8
67 Pesticides Analysis in Avocado by LC and GC-QQQ
November 7, 2015 9
Centrifuge @ 5000 rpm for 5 min
November 7, 2015 10
Add 5 mL of water to EMR dSPE in 15 mL tubes and Add 5 mL of upper ACN extract
Vortex and Centrifuge
Professor Amadeo R. Ferná ndez-Alba Pesticide Residue Research Group, European Union Reference Laboratory (EURL) for pesticides in fruit and vegetables: University of Almerí a.
November 7, 2015 11
Transfer supernatant to EMR polish tube
Vortex, centrifuge, and transfer the upper ACN layer to another vial
November 7, 2015 12
GC-MS Full scan Avocado
November 7, 2015 5
SPE/SLE SEC/GPC
Load and elute Chromatographic separation
d-SPE
2015年8月11日全球推出 NEW d-SPE material for fatty samples
QuEChERS
EMR-Lipid
牛肝脏中兽药多残留分析
November 7, 2015 17
November 7, 2015 18
Method Accuracy and Precision
November 7, 2015 19
Targeted Lipids: - Fatty acids - Glycerolipids - Glycerophospholipids - Sphingolipids - Saccharolipids
Sample Preparation —— SPE, QuEChERS, EMR-Lipid Chromatographic Separation—— UHPLC, SFC Qualitative Analysis —— PCDL, MSC, All Ion MS/MS
Quantitative Analysis —— QTOF
安捷伦液质联用技术平台
MS-based Strategies in Screening for non-edible substances in food and Foodomics
食品中非食用物质快速筛查及食品组学
安捷伦科技（中国）有限公司
Topics 主 题
Screening for non-edible substances in food 食品中非食用物质快速筛查
Avocado – Untreated Avocado – EMR Treated
November 7, 2015 13
EMR-Lipid 实现了 92% 的基质去除率
Avocado extract after EMR –lipid cleanup % Matrix removal = 92%
November 7, 2015 14
November 7, 2015 4
Current Procedures for Lipid Removal
Method
Dilute and Shoot Protein Precipitation
Lipid Removal
No lipid removal PPT followed by centrifugation PPT followed by filtration with or without sorbent
Foodomics 食品组学
November 7, 2015 2
5990-4917CHCN Agilent’s SPE Food Safety Applications Notebook
5990-8593CHCN Sample Preparation Application Guide
5990-4977CHCN Agilent’s Bond Elut QuEChERS Food Safety Applications Notebook
November 7, 2015 20
Sample Preparation —— SPE, QuEChERS, EMR-Lipid Chromatographic Separation—— UHPLC, SFC Qualitative Analysis —— PCDL, MSC, All Ion MS/MS Quantitative Analysis —— QTOF
• • • • • • •
分析型 SFC 系统
SFC 性能和灵敏度与传统的LC-一致 600 bar x 5 mL/min 大量程范围 3 x 倍快于 LC (源于CO2的高扩散系数) 10-15x 倍的低成本和低消耗 绿色环保 业内成熟的1200 Infinity 平台 适合多种检测器 UV, ELSD, MS • • • •
November 7, 2015 23
Where SFC Fits In: from non-polar to highly-charged
November 7, 2015 24
现代SFC仪器设计上与HPLC仪器相似
CO2 气体被液化、加压
改性剂放在泵的B通道， 通常使用醇类： • Methanol • Ethanol... 固定定量环的自动进样器
氯苯胺灵
戊菌唑
苯硫膦
Matrix effect (ME): the analyte response (peak area) was compared between post-spiked avocado extracts and the equivalent neat solutions.
November 7, 2015 15
SFC/UHPLC Hybrid System
1260 Infinity 分析型 SFC 液相色谱泵（四元或两元） 2 位 / 10 通阀 SFC/UHPLC 组件
最经济
最佳的 SFC 性能
SFC 与 UHPLC 互相转换 正交互补的分离能力
November 7, 2015 26
Advantages of Hybrid SFC/UHPLC System
15 g comminuted Avocado sample in 50 mL centrifuge tube
Add 15 mL of 1% Acetic Acid in Acetonitrile and AOAC QuEChERS extraction kit
Cap and shake vigorously on mechanical shaker for 2 min
Method Accuracy and Precision
November 7, 2015 16
Veterinary Drugs in Bovine Liver GC-MS Full scan Beef Liver
Beef Liver – Untreated Beef Liver – EMR Treated
November 7, 2015 21
UHPLC: Fast, High Resolution Separation
HPLC •70mL •114bar
70min
UHPLC •5.6mL •520 bar
14min
November 7, 2015 22
Supercritical fluid chromatography-mass spectrum SFC-MS
Agilent Innovation: Enhanced Matrix Removal
EMR: As easy to use as QuEChERS As clean as SPE
November 7, 2015 6
EMR-Lipid 产品
Activated with water • Creates a large surface area that interacts and traps matrix interferences (aliphatic carbon chains) • Centrifugation removes the matrix/particles
CO2 气体
耐高压流动池 调节反压使流体 CO2再变为气态 Waste
SFC和HPLC一样简单，CO2 as mobile phase
SFC级液态CO2 标准气态CO2
November 7, 2015 25
安捷伦使客户更容易获得SFC分析能力 … …
从 HPLC 升级到 SFC
• Fusion A5 • 1260 SFC binary pump • SFC accessory kit 把现有 1100/1200 转为 SFC
Not selective; insufficient lipid removal; analyte loss
Low total lipid capacity; analyte recovery Time needed; loss of analyte Time needed; solvent usage; extensive method development Uses copious amounts of solvent and time; capital expense
安捷伦SFC/UHPLC 组合系统(Hybrid System)的优势
• Obtain complementary data on analyte mixtures in a single sequence of runs by switching between SFC and UHPLC mode on a single instrument
Weakness
No lipid removal Insufficient lipid removal Insufficient lipid removal; low analyte recovery
QuEChERS
PSA/C18 sorbent Zr-containing sorbent Freeze sample
• • 大幅度节省用户购买两台系统的花费 高效方便，省时、省钱，还节省空间！
• 安捷伦是唯一能够在同一系统提供两种技术的公司
November 7, 2Baidu Nhomakorabea15 27
November 7, 2015 3
The challenges of QuEChERS
QuEChERS方法适用于低脂肪含量的基质，如大部份的水果蔬 菜。应用在高脂肪含量基质时，一般需要略作调整
high fat matrixes
“Even small amounts of lipids can damage the column, source and detector. Fatty acids also interfere with the analysis…. They can produce broad peaks which overlap analyte peaks and can also increase matrix effects.”
一个样品序列可在SFC 与 LC之间相互切换 LC 与 SFC之间无需平衡 无需仪器变化即可直接进行SFC 与 LC 的结果比较 Simply switch the valve
• Save significant cost and laboratory space
November 7, 2015 7
牛油果中脂肪含量达20%！
Pesticides in Avocado
牛油果中的农残
November 7, 2015 8
67 Pesticides Analysis in Avocado by LC and GC-QQQ
November 7, 2015 9
Centrifuge @ 5000 rpm for 5 min
November 7, 2015 10
Add 5 mL of water to EMR dSPE in 15 mL tubes and Add 5 mL of upper ACN extract
Vortex and Centrifuge
Professor Amadeo R. Ferná ndez-Alba Pesticide Residue Research Group, European Union Reference Laboratory (EURL) for pesticides in fruit and vegetables: University of Almerí a.
November 7, 2015 11
Transfer supernatant to EMR polish tube
Vortex, centrifuge, and transfer the upper ACN layer to another vial
November 7, 2015 12
GC-MS Full scan Avocado
November 7, 2015 5
SPE/SLE SEC/GPC
Load and elute Chromatographic separation
d-SPE
2015年8月11日全球推出 NEW d-SPE material for fatty samples
QuEChERS
EMR-Lipid
牛肝脏中兽药多残留分析
November 7, 2015 17
November 7, 2015 18
Method Accuracy and Precision
November 7, 2015 19
Targeted Lipids: - Fatty acids - Glycerolipids - Glycerophospholipids - Sphingolipids - Saccharolipids
Sample Preparation —— SPE, QuEChERS, EMR-Lipid Chromatographic Separation—— UHPLC, SFC Qualitative Analysis —— PCDL, MSC, All Ion MS/MS
Quantitative Analysis —— QTOF
安捷伦液质联用技术平台
MS-based Strategies in Screening for non-edible substances in food and Foodomics
食品中非食用物质快速筛查及食品组学
安捷伦科技（中国）有限公司
Topics 主 题
Screening for non-edible substances in food 食品中非食用物质快速筛查
Avocado – Untreated Avocado – EMR Treated
November 7, 2015 13
EMR-Lipid 实现了 92% 的基质去除率
Avocado extract after EMR –lipid cleanup % Matrix removal = 92%
November 7, 2015 14
November 7, 2015 4
Current Procedures for Lipid Removal
Method
Dilute and Shoot Protein Precipitation
Lipid Removal
No lipid removal PPT followed by centrifugation PPT followed by filtration with or without sorbent
Foodomics 食品组学
November 7, 2015 2
5990-4917CHCN Agilent’s SPE Food Safety Applications Notebook
5990-8593CHCN Sample Preparation Application Guide
5990-4977CHCN Agilent’s Bond Elut QuEChERS Food Safety Applications Notebook
November 7, 2015 20
Sample Preparation —— SPE, QuEChERS, EMR-Lipid Chromatographic Separation—— UHPLC, SFC Qualitative Analysis —— PCDL, MSC, All Ion MS/MS Quantitative Analysis —— QTOF
• • • • • • •
分析型 SFC 系统
SFC 性能和灵敏度与传统的LC-一致 600 bar x 5 mL/min 大量程范围 3 x 倍快于 LC (源于CO2的高扩散系数) 10-15x 倍的低成本和低消耗 绿色环保 业内成熟的1200 Infinity 平台 适合多种检测器 UV, ELSD, MS • • • •
November 7, 2015 23
Where SFC Fits In: from non-polar to highly-charged
November 7, 2015 24
现代SFC仪器设计上与HPLC仪器相似
CO2 气体被液化、加压
改性剂放在泵的B通道， 通常使用醇类： • Methanol • Ethanol... 固定定量环的自动进样器
氯苯胺灵
戊菌唑
苯硫膦
Matrix effect (ME): the analyte response (peak area) was compared between post-spiked avocado extracts and the equivalent neat solutions.
November 7, 2015 15
SFC/UHPLC Hybrid System
1260 Infinity 分析型 SFC 液相色谱泵（四元或两元） 2 位 / 10 通阀 SFC/UHPLC 组件
最经济
最佳的 SFC 性能
SFC 与 UHPLC 互相转换 正交互补的分离能力
November 7, 2015 26
Advantages of Hybrid SFC/UHPLC System
15 g comminuted Avocado sample in 50 mL centrifuge tube
Add 15 mL of 1% Acetic Acid in Acetonitrile and AOAC QuEChERS extraction kit
Cap and shake vigorously on mechanical shaker for 2 min
Method Accuracy and Precision
November 7, 2015 16
Veterinary Drugs in Bovine Liver GC-MS Full scan Beef Liver
Beef Liver – Untreated Beef Liver – EMR Treated
November 7, 2015 21
UHPLC: Fast, High Resolution Separation
HPLC •70mL •114bar
70min
UHPLC •5.6mL •520 bar
14min
November 7, 2015 22
Supercritical fluid chromatography-mass spectrum SFC-MS
Agilent Innovation: Enhanced Matrix Removal
EMR: As easy to use as QuEChERS As clean as SPE
November 7, 2015 6
EMR-Lipid 产品
Activated with water • Creates a large surface area that interacts and traps matrix interferences (aliphatic carbon chains) • Centrifugation removes the matrix/particles
CO2 气体
耐高压流动池 调节反压使流体 CO2再变为气态 Waste
SFC和HPLC一样简单，CO2 as mobile phase
SFC级液态CO2 标准气态CO2
November 7, 2015 25
安捷伦使客户更容易获得SFC分析能力 … …
从 HPLC 升级到 SFC
• Fusion A5 • 1260 SFC binary pump • SFC accessory kit 把现有 1100/1200 转为 SFC
Not selective; insufficient lipid removal; analyte loss
Low total lipid capacity; analyte recovery Time needed; loss of analyte Time needed; solvent usage; extensive method development Uses copious amounts of solvent and time; capital expense
安捷伦SFC/UHPLC 组合系统(Hybrid System)的优势
• Obtain complementary data on analyte mixtures in a single sequence of runs by switching between SFC and UHPLC mode on a single instrument
Weakness
No lipid removal Insufficient lipid removal Insufficient lipid removal; low analyte recovery
QuEChERS
PSA/C18 sorbent Zr-containing sorbent Freeze sample
• • 大幅度节省用户购买两台系统的花费 高效方便，省时、省钱，还节省空间！
• 安捷伦是唯一能够在同一系统提供两种技术的公司
November 7, 2Baidu Nhomakorabea15 27
November 7, 2015 3
The challenges of QuEChERS
QuEChERS方法适用于低脂肪含量的基质，如大部份的水果蔬 菜。应用在高脂肪含量基质时，一般需要略作调整
high fat matrixes
“Even small amounts of lipids can damage the column, source and detector. Fatty acids also interfere with the analysis…. They can produce broad peaks which overlap analyte peaks and can also increase matrix effects.”