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
10期
3000-3007
,共8页
黄娟%张晓燕%刘艳%沈伟健%张睿%沈崇钰%吴斌%陈惠兰%张健%殷耀
黃娟%張曉燕%劉豔%瀋偉健%張睿%瀋崇鈺%吳斌%陳惠蘭%張健%慇耀
황연%장효연%류염%침위건%장예%침숭옥%오빈%진혜란%장건%은요
赭曲霉毒素A%蜂花粉%固相萃取%高效液相色谱-串联质谱法
赭麯黴毒素A%蜂花粉%固相萃取%高效液相色譜-串聯質譜法
자곡매독소A%봉화분%고상췌취%고효액상색보-천련질보법
ochratoxin A%bee pollen%solid phase extraction%high performance liquid chromatography- tandem mass spectrometry
目的：建立蜂花粉中赭曲霉毒素A(ochratoxin A, OTA)的高效液相色谱-串联质谱(HPLC-MS/MS)检测方法。方法样品经乙腈提取,固相萃取柱富集净化后,采用 HPLC-MS/MS 对目标物进行定性确证和定量分析。在Leapsil C18(100 mm×3.0 mm,2.7μm)上以0.005 mol/L乙酸铵甲酸水溶液和乙腈为流动相进行梯度洗脱分离；质谱采集模式为电喷雾负离子监测模式。结果本方法的赭曲霉毒素A的定量限(以S/N=10计)为5μg/kg；在5～100μg/L的质量浓度范围内呈现良好的线性关系,相关系数(r)大于0.99。本底空白的玉米花粉、茶花粉、荷花粉、油菜花粉4种基质中5、10、20μg/kg添加水平下的加标回收率范围为84.6%～103.6%,精密度范围为5.1%～12.2％。结论本方法准确可靠、灵敏度高、经济实用,可替代较为昂贵的免疫亲和柱,较大降低检测成本,且适用于大部分蜂花粉基质的测定。
目的：建立蜂花粉中赭麯黴毒素A(ochratoxin A, OTA)的高效液相色譜-串聯質譜(HPLC-MS/MS)檢測方法。方法樣品經乙腈提取,固相萃取柱富集淨化後,採用 HPLC-MS/MS 對目標物進行定性確證和定量分析。在Leapsil C18(100 mm×3.0 mm,2.7μm)上以0.005 mol/L乙痠銨甲痠水溶液和乙腈為流動相進行梯度洗脫分離；質譜採集模式為電噴霧負離子鑑測模式。結果本方法的赭麯黴毒素A的定量限(以S/N=10計)為5μg/kg；在5～100μg/L的質量濃度範圍內呈現良好的線性關繫,相關繫數(r)大于0.99。本底空白的玉米花粉、茶花粉、荷花粉、油菜花粉4種基質中5、10、20μg/kg添加水平下的加標迴收率範圍為84.6%～103.6%,精密度範圍為5.1%～12.2％。結論本方法準確可靠、靈敏度高、經濟實用,可替代較為昂貴的免疫親和柱,較大降低檢測成本,且適用于大部分蜂花粉基質的測定。
목적：건립봉화분중자곡매독소A(ochratoxin A, OTA)적고효액상색보-천련질보(HPLC-MS/MS)검측방법。방법양품경을정제취,고상췌취주부집정화후,채용 HPLC-MS/MS 대목표물진행정성학증화정량분석。재Leapsil C18(100 mm×3.0 mm,2.7μm)상이0.005 mol/L을산안갑산수용액화을정위류동상진행제도세탈분리；질보채집모식위전분무부리자감측모식。결과본방법적자곡매독소A적정량한(이S/N=10계)위5μg/kg；재5～100μg/L적질량농도범위내정현량호적선성관계,상관계수(r)대우0.99。본저공백적옥미화분、다화분、하화분、유채화분4충기질중5、10、20μg/kg첨가수평하적가표회수솔범위위84.6%～103.6%,정밀도범위위5.1%～12.2％。결론본방법준학가고、령민도고、경제실용,가체대교위앙귀적면역친화주,교대강저검측성본,차괄용우대부분봉화분기질적측정。
Objective To establish a method for the determination of ochratoxin A in pollen based on high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS).Methods The sample was extracted by acetonitrileand cleaned up by solid phase extraction cartridge. The separation was carried out on a Leapsil C18(100 mm×3.0 mm, 2.7 μm) with a gradient elution using 0.005 mol/L ammonium acetate formic acid solution and acetonitrile as mobile phases. The analysis of ochratoxin A was performed under electrospray negative ionization mode.Results The limits of quantification (LOQ, S/N=10) was 5μg/kg. A good linearity (r >0.99) was achieved for the target compounds over the range of 5~100μg/L. The recoveries at the three spiked levels (5, 10, 20μg/kg) in the blank matrices such as corn pollen, camellia pollen, lotus pollen, and rape pollen, were varied from 84.6% to103.6% with the relative standard deviations varied from 5.1% to 12.2%. Conclusion The method is accurate, efficient, sensitive and practical. The cost of detection is obviously re-duced by replacing immunoaffinity column with HLB column which has the same purification effect. It can be applied to most of pollen which may be contaminated by Ochratoxin A.
