GB/T 6682-1992

蜂蜜中羥甲基糠醛含量的液相色譜測定方法，檢出限nt face="Times New Roman">1.0mg/kgnt>nt face="宋體">，蜂蜜樣品中的羥甲基糠醛經nt>nt face="Times New Roman">HPLCnt>nt face="宋體">反相色譜柱分離，用液相色譜機紫外檢測器檢測，通過色譜軟件來收集圖譜、查看標準曲線外標法定量。本方法使用我公司nt>STI501系列高效液相色譜機系統來檢測，檢測精度滿足nt face="Times New Roman">GB/T6682-1992nt>nt face="宋體">要求。nt>

1nt face="宋體">檢測條件  nt>

   1.1nt face="宋體">甲醇nt>nt face="Times New Roman">:nt>nt face="宋體">色譜純。nt>

   1.2nt face="宋體">甲醇溶液nt>nt face="Times New Roman">:10%,nt>nt face="宋體">吸取nt>nt face="Times New Roman">100ml,nt>nt face="宋體">的甲醇到nt>nt face="Times New Roman">1000 MLnt>nt face="宋體">的容量瓶中，用水稀釋至刻度。nt>

   1.3nt face="宋體">標準物質nt>nt face="Times New Roman">:nt>nt face="宋體">羥甲基糠醛純度≥nt>nt face="Times New Roman">99%,nt>

   1.4nt face="宋體">標準儲備溶液nt>nt face="Times New Roman">:nt>nt face="宋體">準確稱取適量的羥甲基糠醛標準物質於nt>nt face="Times New Roman">100mLnt>nt face="宋體">容量瓶，用nt>nt face="Times New Roman">10ml,nt>nt face="宋體">甲醇溶解，用水稀釋至刻度，配成nt>nt face="Times New Roman">0.20mg/mLnt>nt face="宋體">的標準儲備液。此溶液可在溫度低於nt>nt face="Times New Roman">4nt>nt face="宋體">℃冰箱中冷藏保存兩個月。nt>

1.5nt face="宋體">標準工作溶液nt>nt face="Times New Roman">:nt>nt face="宋體">分別吸取適量的羥甲基糠醛標準儲備溶液至nt>nt face="Times New Roman">100mLnt>nt face="宋體">容量瓶中，用nt>nt face="Times New Roman">10%nt>nt face="宋體">甲醇溶液釋稀至刻度，配成nt>nt face="Times New Roman">0.10ug/mLnt>nt face="宋體">，nt>nt face="Times New Roman">0.20ug/mLnt>nt face="宋體">，nt>nt face="Times New Roman">1.0ug/mLnt>nt face="宋體">，nt>nt face="Times New Roman">2.0ug/mLnt>nt face="宋體">，nt>nt face="Times New Roman">4.0ug/mLnt>nt face="宋體">，nt>nt face="Times New Roman">6.0ug/mLnt>nt face="宋體">，nt>nt face="Times New Roman">10ug/ml,nt>nt face="宋體">標準工作溶液nt>

   2nt face="宋體">機器nt>

2.1501nt face="宋體">高效液相色譜機（杭州賽析科技）nt>:nt face="宋體">配全波長紫外檢測器。nt>

  恒流泵：耐壓nt face="Times New Roman">42Mpant>nt face="宋體">，流速精度nt>nt face="Times New Roman">0.001ml/minnt>

  內置式專用色譜軟件，可做外標法，能兼容nt face="Times New Roman">XPnt>nt face="宋體">操作系統，nt>nt face="Times New Roman">RS-232nt>nt face="宋體">接口nt>

   2.2nt face="宋體">分析天平nt>nt face="Times New Roman">:nt>nt face="宋體">感量nt>nt face="Times New Roman">0.01g,nt>

   2.3nt face="宋體">註射器nt>nt face="Times New Roman">:10mLnt>nt face="宋體">，微量進樣器nt>

2.4nt face="宋體">過濾膜nt>nt face="Times New Roman">:0.45umnt>nt face="宋體">，一次性針式過濾器nt>

2.5 XO-80超音波清洗器、FB-10T溶劑過濾器、nt face="Times New Roman">AP-01nt>nt face="宋體">真空泵nt>

2.6nt face="宋體">色譜柱溫箱nt>

3nt face="宋體">試樣制備與保存nt>

   3.1nt face="宋體">試樣的制備nt>

       無論有無結晶的實驗室樣品，都不要加熱。將其攪拌均勻，分出nt face="Times New Roman">0.5kgnt>nt face="宋體">作為試樣。制備好的試樣置於樣品瓶中，密封，並做上標記。nt>

   3.2nt face="宋體">試樣的保存nt>

       將試樣於室溫下保存。

   4nt face="宋體">測定步驟nt>

   4.1nt face="宋體">試樣處理nt>

       稱取nt face="Times New Roman">10gnt>nt face="宋體">試樣，精確至nt>nt face="Times New Roman">0.01gnt>nt face="宋體">，置於nt>nt face="Times New Roman">100mLnt>nt face="宋體">燒杯中，加人nt>nt face="Times New Roman">10mLnt>nt face="宋體">甲醇nt>nt face="Times New Roman">(1.2)nt>nt face="宋體">，用玻璃棒輕輕攪拌均勻，使試樣完全溶解。轉移至nt>nt face="Times New Roman">l00mLnt>nt face="宋體">容量瓶中，用水釋稀至刻度，充分混勻。用nt>nt face="Times New Roman">0.45u mnt>nt face="宋體">的濾膜過濾，濾液用於液相色譜機紫外檢測器測定。nt>

   4.2nt face="宋體">色譜側定nt>

   4.3nt face="宋體">液相色譜條件nt>

       a)nt face="宋體">色譜柱nt>nt face="Times New Roman">:nt>Vertex C18 5um,250mmX4.6 mm（nt face="Times New Roman">i.d )nt>nt face="宋體">或相當者（美國進口）nt>nt face="Times New Roman">;nt>

       b)nt face="宋體">流動相nt>nt face="Times New Roman">:nt>nt face="宋體">甲醇nt>nt face="Times New Roman">+nt>nt face="宋體">水nt>nt face="Times New Roman">(10nt>nt face="宋體">十nt>nt face="Times New Roman">90);nt>

       c)nt face="宋體">流速nt>nt face="Times New Roman">:1.0 m L/min;nt>

       d)nt face="宋體">檢測波長nt>nt face="Times New Roman">:285n m;nt>

       e)nt face="宋體">柱溫nt>nt face="Times New Roman">:30nt>nt face="宋體">度nt>

       f)nt face="宋體">進樣量nt>nt face="Times New Roman">:10uL.nt>

nt face="Times New Roman">nt> 

4.4nt face="宋體">液相色譜測定nt>

       首先測定七個標準工作溶液nt face="Times New Roman">(1.5)nt>nt face="宋體">在上述色譜條件下的峰麵積，以峰麵積對相應濃度繪制標準工作曲線，然後測定未知樣品，用標準工作曲線對樣品進行定量。樣品溶液中羥甲基糠醛的響應值應在機器的線性范圍內。在上述色譜條件下，羥甲基糠醛的參考保留時間約為nt>nt face="Times New Roman">12 minnt>nt face="宋體">。羥甲基糠醛標準物質色譜圖和含有短甲基糠醛的蜂蜜樣品色譜圖參見附錄nt>nt face="Times New Roman">Ant>nt face="宋體">中圖nt>nt face="Times New Roman">A.1nt>nt face="宋體">、圖nt>nt face="Times New Roman">A.2 ,nt>

   4.5nt face="宋體">平行試驗nt>

       按上述步驟，對同一試樣進行平行試驗測定。

   4.6nt face="宋體">空白試驗nt>

       按上述步驟，對nt face="Times New Roman">10%nt>nt face="宋體">的甲醇溶液進行測定。nt>

   4.7nt face="宋體">添加試驗nt>

       每批樣品應至少進行一個樣品的添加試驗。稱取nt face="Times New Roman">10gnt>nt face="宋體">試樣，精確至nt>nt face="Times New Roman">0.0lgnt>nt face="宋體">，添加nt>nt face="Times New Roman">1.0mLnt>nt face="宋體">羥甲基糠醛標準儲備溶液，加nt>nt face="Times New Roman">9.9mLnt>nt face="宋體">甲醇溶解，其他步驟按試樣處理步驟進行。nt>

   5nt face="宋體">精度nt>

      本部分的精密度數據是按照nt face="Times New Roman">GB/T6379nt>nt face="宋體">的規定確定的，其重復性和再現性的值是以nt>nt face="Times New Roman">95%nt>nt face="宋體">的可信度來計算。nt>

   本方法中經甲基糠醛添加濃度及其回收率的試驗數據nt face="Times New Roman">:nt>

   在添加量為nt face="Times New Roman">1.0mg/kgnt>nt face="宋體">時，平均回收率為nt>nt face="Times New Roman">93.78%;nt>

   在添加量為nt face="Times New Roman">10.0mg/kgnt>nt face="宋體">時，平均回收率為nt>nt face="Times New Roman">94.88%;nt>

   在添加量為nt face="Times New Roman">40.0mg/kgnt>nt face="宋體">時，平均回收率為nt>nt face="Times New Roman">95.76%;nt>

   在添加量為nt face="Times New Roman">100mg/kgnt>nt face="宋體">時，平均回收率為nt>nt face="Times New Roman">94.68%.nt>

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