Investigation Of Detection Approach Of SPE-HPLC Of PAHs In Smoking Meat Products

In this research,a novel chromatographic analysis method is established to analyze polycyclic aromatic hydrocarbons(PAHs)in smoking meat products by combining solid-phase extraction technology(SPE)with high performance liquid chromatography(HPLC),aiming to overcome the defects in general method detecting PAHs in smoking meat products analysis such as:solvent toxicity,bio-hazard.this method is proved to meet the basic demand of PAHs analysis and possesses high recovery rate,less-time cost,good repeatability and feasibility.By using SPE to pre-treat for smoking meat products,then using diode array detecter(PDA)to detect the PAHs in the sample,the result showed that this method is feasible,exact and precise.The conclusions in this paper were mainly as follow:(1)In this thesis,used commercial SPE column,filling with C₁₈,Florisil,alkali aluminum oxide and silica gel,by comparing the recovery rate of the four absorbent,the recovery rate of C₁₈is 80.7%～100.5%,the other three absorbent is 24.2～58.4%,20.5～52.5%,10.6～39.4%respectively. The total absorbent rate of C₁₈to sixteen PAHs is 98.2%.and the tatal absorbent rate of other three SPE columns to sixteen PAHs is 54.7%,48.9%,37.2%respectively.The coefficienr of variation of the four SPE columns is 1.17%～3.07%,0.63%～3.02%,1.09%～3.12%respectively.So,C18 column have more rxtraction effect for PAHs in smoking meat products.(2)When using C₁₈pole to pre-treat the PAHs,the eluting effects among dichloromethane, methanol,acetonitrile and tetrahydrofuran have been compared.The recycle rate is 85.0%～98.7%,15.9%～87.9%,56.0%～77.3%,11.0%～39.3%respectively.So the dichloromethane have most eluting effect for PAHs in C₁₈,and the eluting effect of tetrahydrofuran is the poorest.The volume of elute is 10 ml.(3)The operating condition of chromatogram has been optimized.The chromatogram pole is Hypersil BDS 250mm×4.6mm×5um C₁₈reversed phase High-efficiency Liquid Chromatography column.The mobile phase is acetonitrile and water,The detector is PDA;the quantificational wavelength is 254 nm,;the velocity of flow is 1.0mL/min;the volume of injection sample is 20μl; the temperature of pillar is 30℃.when the range concention is 0.01～2μg/mL,the correlation coefficient is 0.9962～0.9997,The all relative standard deviation is less than 1%.(5)The feasibility of SPE-HPLC method are validated by standard appending 60ng/mL, 100ng/mL,and 1μg/mL respectively in smoking meat products,in this way,when the concentration is 60ng/mL,the recovery rate is between 69.5%and 95.4%,correlation coefficient is between 2.1% and 4.1%;when the concentration is 100ng/mL,the recovery is between 70.8%and 97.4%, correlation coefficient is 1.4%to 4.8%;and when the concentration is 1μg/mL,the recovery is 77.2% to 102.5%,correlation coefficient is 1.6%to 4.0%,Based on those experiment results,showed that the exact,precise and sensitive of the method of soxhlet extraction,cyclohexane extraction and SPE-HPLC can meet the PAHs in smoking meat products analytical demand.(6)The analysis of the PAHs in smoking meat products:Using the method of SPE-HPLC to detect the PAHs in smoking pig's meat products,the results showed that 15 kinds of PAHs have been detected in the sample from GUIZHOU,the kinds of PAHs was less in the sample from CHONGQING,many mixed apex have been detected in the sample from SICHUAN and HUNAN,which would absorbed other substance in fumigate process.In the 16 samples,the content of naphthalene was high,account for 29.46%of the total contention of its,fluorene and phenanthrene accounted for 11.67%and 11.16%respectively.Considering the structure of the PAHs, the three-ring PAHs accounted for 44.7%of the total PAHs,and the two-ring PAHs was second which accounted for 27.7%.The analysis to five carcinogenic PAHs,showed that the average content of benzo[g,h,i]anthracene was the highest,which is 0.99125μg/kg,dibenz[a,h]anthracene was second,which is 0.895625μg/kg,benzo[a]pyrene was lowest,which is O.019375μg/kg,all lower the regulated the most content 5μg/kg by china,and lower contention of benzo[a]pyrene 1μg/kg which is regulated lowest standard in meat products by foreign countries.Using the method of SPE-HPLC to detect the PAHs in smoking banger's meat products also, which came from four different area in CHONGQING.In smoking banger meat products,fourteen kinds of PAHs have detected.In the four samples,the content of naphthalene was high,account for 28.9%,benza[a]anthracene and benza[b]fluoranthene can detected in three samples,and their average content is 1.065μg/kg and 0.22μg/kg respectively.Only one smoking banger meat products contained benzo[a]pyrene,its content is 0.024μg/kg,all lower the regulated the most content 5μg/ kg by china.