食品安全质量检测学报
食品安全質量檢測學報
식품안전질량검측학보
FOOD SAFETY AND QUALITY DETECTION TECHNOLOGY
2014年
9期
2682-2688
,共7页
张建莹%肖锋%叶刚%岳振峰%罗耀%邓慧芬
張建瑩%肖鋒%葉剛%嶽振峰%囉耀%鄧慧芬
장건형%초봉%협강%악진봉%라요%산혜분
荧光增白剂%超高效液相色谱-串联质谱法%固相萃取%食用菌
熒光增白劑%超高效液相色譜-串聯質譜法%固相萃取%食用菌
형광증백제%초고효액상색보-천련질보법%고상췌취%식용균
fluorescent whitening agents%ultra performance liquid chromatography-tandem mass spectrometry%solid phase extraction%edible mushrooms
目的:建立新鲜食用菌中荧光增白剂85(fluorescent brightener VBL, VBL)、荧光增白剂71(fluorescent brightener CXT, CXT)和荧光增白剂113(blankophor BA, BA)的超高效液相色谱-串联质谱(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS,)定量检测方法。方法采用60%甲醇-水溶液,75℃水浴振荡提取试样中的荧光增白剂,经弱阴离子交换固相萃取柱净化,采用UPLC-MS/MS在负离子模式下检测,内标法定量。结果该方法在0.0100~0.500 mg/L范围内有良好的线性关系,相关系数r2>0.990,在空白新鲜食用菌基质中,不同添加水平下方法的平均回收率范围为80.0%~101%,相对标准偏差为3.4%~11.9%;测定低限为0.100 mg/kg。结论此方法灵敏度高、准确、重现性好,适用于新鲜食用菌中荧光增白剂85、荧光增白剂71和荧光增白剂113的检测。
目的:建立新鮮食用菌中熒光增白劑85(fluorescent brightener VBL, VBL)、熒光增白劑71(fluorescent brightener CXT, CXT)和熒光增白劑113(blankophor BA, BA)的超高效液相色譜-串聯質譜(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS,)定量檢測方法。方法採用60%甲醇-水溶液,75℃水浴振盪提取試樣中的熒光增白劑,經弱陰離子交換固相萃取柱淨化,採用UPLC-MS/MS在負離子模式下檢測,內標法定量。結果該方法在0.0100~0.500 mg/L範圍內有良好的線性關繫,相關繫數r2>0.990,在空白新鮮食用菌基質中,不同添加水平下方法的平均迴收率範圍為80.0%~101%,相對標準偏差為3.4%~11.9%;測定低限為0.100 mg/kg。結論此方法靈敏度高、準確、重現性好,適用于新鮮食用菌中熒光增白劑85、熒光增白劑71和熒光增白劑113的檢測。
목적:건립신선식용균중형광증백제85(fluorescent brightener VBL, VBL)、형광증백제71(fluorescent brightener CXT, CXT)화형광증백제113(blankophor BA, BA)적초고효액상색보-천련질보(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS,)정량검측방법。방법채용60%갑순-수용액,75℃수욕진탕제취시양중적형광증백제,경약음리자교환고상췌취주정화,채용UPLC-MS/MS재부리자모식하검측,내표법정량。결과해방법재0.0100~0.500 mg/L범위내유량호적선성관계,상관계수r2>0.990,재공백신선식용균기질중,불동첨가수평하방법적평균회수솔범위위80.0%~101%,상대표준편차위3.4%~11.9%;측정저한위0.100 mg/kg。결론차방법령민도고、준학、중현성호,괄용우신선식용균중형광증백제85、형광증백제71화형광증백제113적검측。
Objective To establish an ultra performance liquid chromatography-tandem mass spectrometry method for the determination of three fluorescent whitening agents (fluorescent brightener VBL, fluorescent brightener CXT and blankophor BA) in edible mushrooms. Methods The residues of fluorescent whitening agents in the test samples were extracted with 60% methanol water solution by a 75 ℃ shaking water bath. After being cleaned up with weak anion exchange solid-phase extraction column, the residues were detected by ultra performance liquid chromatography-tandem mass spectrometry under multiple reactions monitoring (MRM) mode via negative-ion mode and quantified by an internal standard method. Results The method showed a good linearity over the range of 0.0100~0.500 mg/L for three fluorescent whitening agents with r2>0.990. The average recoveries were 80.0%~101% at three spiked levels in edible mushrooms and the relative standard deviations were 3.4%~11.9%. The limit of quantitation was 0.100 mg/kg. Conclusion This method was highly sensitive, accurate and reproducible, and it could be suitable for the detection of three fluorescent whitening agents VBL, CXT and BA in edible mushrooms.