使用頂空氣相層析質譜法與通氣蒸餾法檢測食品中二氧化硫殘留量

Determination of Sulfur Dioxide Residues in Food by Headspace-Gas Chromatography Mass Spectrometry and Aeration Distillation

張凱婷(Kai-Ting Chang) ； 葉淑幸(Shu-Xing Yeh)

《檢驗及品保雜誌》 11卷2期 (2022/04) Pp. 48-56

https://doi.org/10.6573/JTQA.202204_11(2).02

摘要

食品中的二氧化硫來自於亞硫酸鹽類，是合法的食品添加物，其具有漂白、防腐、殺菌及抑制氧化等優點。現今衛生福利部食品藥物管理署（TFDA）檢驗食品中二氧化硫殘留量之公告方法為通氣蒸餾法，另外TFDA亦於2017年公告一建議檢測方法－食品中二氧化硫檢驗方法（氣相層析質譜法），其係以頂空進樣系統結合氣相層析質譜儀（headspace-gas chromatography mass spectrometry, HS-GC-MS）。本研究以此建議方法為基礎，修飾部份分析條件，並使用空白基質－山藥粉添加不同濃度的二氧化硫進行分析方法各項參數的確效評估，結果指出HS-GC-MS 法具有專一性，標準曲線濃度範圍為5～250 g/mL，線性迴歸相關係數（R）可達0.999。添加三種不同濃度的二氧化硫標準溶液至空白基質－山藥粉中，其平均回收率（n=5）介於84.73%～103.80%，變異係數CV（%）低於10%，且Intra-day及Inter-day之重複性精密度與中間精密度（n=6）測試之變異係數CV（%）值皆低於10%，均符合確效規範。接著利用經確效的HS-GC-MS法檢測市售產品：酸菜、白葡萄酒與乾燥金針之二氧化硫殘留量，其樣品二重複檢測之相對差異百分比（relative percent difference, RPD）分別為5.88%、0.58%與3.18%；使用通氣蒸餾法檢測樣品二重複之相對差異百分比分別為10.62%、5.87%與7.33%。進一步確認此方法於不同樣品之回收率，分別添加二氧化硫標準溶液50 g/g至已確認樣品濃度之三種不同基質中，其HS-GC-MS法之平均回收率（n=2）分別為96.11%、85.53%與94.64%；通氣蒸餾法之平均回收率（n=2）分別為76.35%、85.08%與78.73%。綜合以上結果顯示HS-GC-MS法較不易受基質干擾及人為因素影響而造成檢驗結果之誤差。

關鍵字

二氧化硫 ； 亞硫酸鹽 ； 頂空 ； 氣相層析質譜儀 ； 通氣蒸餾法

並列摘要

Sulfur dioxide in food is derived from sulfites that are commonly used as food additives for bleaching and prevention of spoilage, bacterial growth, and oxidation. Aeration distillation has been the standard method recommended by Taiwan FDA (TFDA) for detection of sulfur dioxide in food for many years. In 2017, TFDA recommended headspace-gas chromatography mass spectrometry (HS-GC-MS) as an alternative method. In this study, we compared the efficacy of these two methods in the detection of sulfur dioxide. To evaluate HS-GC-MS, a standard calibration curve with 5, 10, 20, 50, 100, and 250 g/mL of sulfur dioxide vs. HS-GC-MS counts was first constructed and found to have a correlation coefficient (R) of 0.999, indicating the accuracy of the method. The method was then used to analyzed plain yam flour spiked with various concentrations (10, 25, and 50 g/g) of sulfur dioxide. Results of 5 repeats on each sample showed that the recovery rates of spiked sulfur dioxide were in the range of 84.73% to 103.80% with a coefficient of variation of both intra-day and inter-day less than 10%. To compare its efficiency with that of aeration distillation, both methods were used to detect sulfur dioxide in pickled mustard green, white wine, and dried orange daylily. Each sample was analyzed twice. The amounts sulfur dioxide determined in the two repeats by HS-GC-MS differed by 5.88%, 0.58%, and 3.18%, and those by aeration distillation differed by 10.62%, 5.87%, and 7.33%, respectively, in the 3 kinds of samples. To further evaluate the two methods, pickled mustard green and dried orange daylily samples were spiked with 50 g/g of sulfur dioxide, and the white wine sample was spiked with 50 g/mL of sulfur dioxide. Results showed that the recovery rates of spiked sulfur dioxide in the 3 kinds of samples by HS-GC-MS were 96.11%, 85.53%, and 94.64%, and those by aeration distillation were 76.35%, 85.08% and 78.73%, respectively. Taken together, results of this study indicate that HS-GC-MS is applicable to various kinds of foods and is more sensitive and less prone to technical errors than aeration distillation.

並列關鍵字

Sulfur dioxide ； sulfites ； headspace ； gas-chromatography mass spectrometry ； aeration distillation