以HPLC檢測南投地區市售麵濕製品、米濕製品防腐劑含量研究

Determination of preservative contents from market-available wet noodle products and wet rice products in Nantou Area by HPLC

曾月昭(tseng yueh jan)

指導教授 ： 張竣維

亞洲大學/資訊學院/生物資訊學系碩士班/碩士(2007年)

摘要

為瞭解市售麵濕製品、米濕製品的衛生安全，業者在製造過程中是否有不當添加防腐劑之慮，而危害消費者健康，特針對麵濕製品、米濕製品進行調查，本研究以高效液相層析儀(HPLC)，檢測麵濕製品、米濕製品中防腐劑(包括苯甲酸、己二烯酸及去水醋酸)的含量。 於96年5-11月間抽驗市售麵濕製品41件、米濕製品39件，共計80件。固體樣品以水蒸氣蒸餾抽出法，後以0.45μm濾膜過濾；液體樣品以甲醇與純水（1：1）溶液稀釋後，以0.45μm濾膜過濾後注入HPLC加以分析，HPLC使用SUPELCO C18 15 ㎝ × 4.6 mm(長度) 5μm(內徑)層析管，用甲醇：乙腈：5 mM檸檬酸緩衝液(1：2：7)為移動相，在流速為1 mL/min流完成間15分，於UV 230 nm下檢測苯甲酸、己二烯酸及去水醋酸。線性範圍5 ppm~100 ppm，線性相關係數在 r=1；儀器偵測極限(IDL) ：己二烯酸(sorbic acid) 0.090 ppm、苯甲酸(benzoic acid)0.090 ppm、去水醋酸(dehydroacetic acid) 0.090 ppm；方法偵測極限(MDL)己二烯酸(sorbic acid)0.090 ppm、苯甲酸(benzoic acid)0.093 ppm、去水醋酸(dehydroacetic acid) 0.090 ppm；添加適當混合標準溶液於液體樣品中檢測分析平均回收率分別為：己二烯酸(sorbic acid) 98.380 ％、苯甲酸(BA) 95.222％、去水醋酸(DHA) 97.864 ％； 空白樣品試驗檢出均為0 ；重覆試驗分析平均相對差異百分比：己二烯酸(sorbic acid) 0.926% 、苯甲酸(benzoic acid) 0.996%、去水醋酸(dehydroacetic acid)2.251 %；查核樣品分析平均回收率：己二烯酸(sorbic acid) 101.625%、苯甲酸(benzoic acid)101.107%、去水醋酸(dehydroacetic acid)101.984%。80件市售樣品中，檢測結果有21件樣品的防腐劑超過限量。分別為己二烯酸4件、去水醋酸5件、苯甲酸12件與規定不符(麵食類食品衛生標準不得添加)，總不合格率為26.250﹪，其中麵濕製品類8件，米濕製品類13件。

關鍵字

HASH(0x8b30b7c)

並列摘要

The aim of this study was to ensure the safety of market-available wet noodle products and rice wet products by investigating whether these products were contaminated with food additive or preservative or not. An HPLC system was applied to detect the concentrations of preservatives including sorbic acid, benzoic acid and dehydroacetic acid. In 2007, 41 market-available wet noodle products and 39 wet rice products were randomly selected from May to November for this study.
Solid samples were filtered by 0.45 μm filter after distillation, and liquid samples were diluted with 50% methanol in water, then filtered by 0.45 μm filter before sample injection. The samples were analyzed for sorbic acid, benzoic acid and dehydroacetic acid for 15 min by HPLC. The HPLC system equipped with a Supelco C18 15 cm × 4.6 mm, 5μm column. The mobile phase was methanol：acetonitrile：5 mM citric acid (1: 2: 7). The samples were analyzed with flow rate of 1ml/min and were monitored at λ=230 nm to detect benzoic acid, sorbic acid and dehydroacetic acid. The linear range was from 5 ppm to 100 ppm with correlation coefficient (r )= 1. IDL was 0.090 ppm for benzoic acid, 0.090 ppm for sorbic acid and 0.090 ppm for dehydroacetic acid. MDL was 0.090 ppm for benzoic acid, 0.093 ppm for sorbic acid and 0.090 ppm for dehydroacetic acid. The average recovery of standard spike added to samples were 98.380% for sorbic acid, 95.222% for benzoic acid and 97.864% for dehydroacetic acid. Blank test was 0% after triplicate studies. The average RPD was 0.926% for sorbic acid, 0.996% for benzoic acid, and 2.251% for dehydroacetic acid. The average recovery of standard spike addition were 101.625% for sorbic acid, 101.107% for benzoic acid, and 101.948% dehydroacetic acid.
In conclusion, 21 products out of 80 products including 8 wet noodle samples products and 13 wet rice products were found over the allowable preservative limitations. Four samples were found with sorbic acid, 12 samples were found with benzoic acid, and 5 samples were found with dehydroacetic acid. The total failed rate was 26.25%.

參考文獻

5.行政院衛生署〈2005〉食品添加物使用範圍及用量標準。

7.食品衛生法規彙編，行政院衛生署，2003。

17. 食品衛生法規彙編，行政院衛生署，2003。

4.Z.Giang.“The Secret Sweeten.Delicious food”Taiwan R.O.C.，No.46，1995， 87。

26.M.P.L.V.O.Ferreira ，E.Mendes，P.Brita，M.A.Ferria，“simultaneous Determination of Benzoic and Sorbic acid in Quine Jam by HPLC”Food Research International，33，2000， 113-117。