超高效液相色谱-三重四极杆质谱法测定保健食品中28种降糖类非法添加化合物
目的建立超高效液相色谱一三重四极杆质谱法测定保健食品中28种降糖类非法添加化合物的分析方法。方法采用Merck SeQuantZIC-HILIC色谱柱（100mm×2．1mmTl，3．5μm），以乙腈-含10mmol／L甲酸铵的0．1％甲酸水溶液为流动相梯度洗脱，分离二甲双胍等3种化合物；采用WatersCORTECST3色谱柱（100min×2．1mm，2．7μm），以乙腈．0．1％甲酸水溶液为流动相梯度洗脱，分离苯乙双胍等25种化合物，在电喷雾离子化正离子或负离子模式下，以多反应监测方式（multiple reaction monitoring，MRM）检测。结果二甲双胍等3种化合物在进样...
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| Published in | 食品安全质量检测学报 Vol. 9; no. 1; pp. 93 - 102 |
|---|---|
| Main Author | |
| Format | Journal Article |
| Language | Chinese |
| Published |
上海市食品药品检验所,上海,201203
2018
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| Subjects | |
| Online Access | Get full text |
| ISSN | 2095-0381 |
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| Abstract | 目的建立超高效液相色谱一三重四极杆质谱法测定保健食品中28种降糖类非法添加化合物的分析方法。方法采用Merck SeQuantZIC-HILIC色谱柱（100mm×2．1mmTl，3．5μm），以乙腈-含10mmol／L甲酸铵的0．1％甲酸水溶液为流动相梯度洗脱，分离二甲双胍等3种化合物；采用WatersCORTECST3色谱柱（100min×2．1mm，2．7μm），以乙腈．0．1％甲酸水溶液为流动相梯度洗脱，分离苯乙双胍等25种化合物，在电喷雾离子化正离子或负离子模式下，以多反应监测方式（multiple reaction monitoring，MRM）检测。结果二甲双胍等3种化合物在进样浓度为50～1000pg／L范围内线性关系良好，妥拉磺脲等5种化合物在25～500μg／L范围内线性关系良好，其余20种化合物在5～100gg／L范围内线性关系良好，相关系数（r）均大于0．99。各化合物在定量限（1imit of quantity,LOQ）I倍、2倍、10倍添加水平下的平均加标回收率为48．6％～134．4％，相对标准偏差（relative standar ddeviation，RSD）为0．1％～8．4％（n=6）。二甲双胍等3种化合物的定量限为500μg／kg，妥拉磺脲等5种化合物的定量限为250μg／kg，苯乙双胍等20种化合物的定量限为50μg／kg。结论本方法灵敏、高效，可用于测定保健食品中降糖类非法添加化合物含量。 |
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| AbstractList | 目的 建立超高效液相色谱-三重四极杆质谱法测定保健食品中28种降糖类非法添加化合物的分析方法.方法 采用Merck SeQuant ZIC-HILIC色谱柱(100 mm×2.1 mm,3.5μm),以乙腈-含10 mmol/L甲酸铵的0.1％甲酸水溶液为流动相梯度洗脱,分离二甲双胍等3种化合物;采用Waters CORTECS T3色谱柱(100 mm×2.1 mm,2.7μm),以乙腈-0.1％甲酸水溶液为流动相梯度洗脱,分离苯乙双胍等25种化合物,在电喷雾离子化正离子或负离子模式下,以多反应监测方式(multiple reaction monitoring,MRM)检测.结果 二甲双胍等3种化合物在进样浓度为50～1000μg/L范围内线性关系良好,妥拉磺脲等5种化合物在25～500μg/L范围内线性关系良好,其余20种化合物在5～100μg/L范围内线性关系良好,相关系数(r)均大于0.99.各化合物在定量限(limit of quantity,LOQ)1倍、2倍、10倍添加水平下的平均加标回收率为48.6％～134.4％,相对标准偏差(relative standard deviation,RSD)为0.1％～8.4％(n=6).二甲双胍等3种化合物的定量限为500μg/kg,妥拉磺脲等5种化合物的定量限为250μg/kg,苯乙双胍等20种化合物的定量限为50μg/kg.结论 本方法灵敏、高效,可用于测定保健食品中降糖类非法添加化合物含量. 目的建立超高效液相色谱一三重四极杆质谱法测定保健食品中28种降糖类非法添加化合物的分析方法。方法采用Merck SeQuantZIC-HILIC色谱柱（100mm×2．1mmTl，3．5μm），以乙腈-含10mmol／L甲酸铵的0．1％甲酸水溶液为流动相梯度洗脱，分离二甲双胍等3种化合物；采用WatersCORTECST3色谱柱（100min×2．1mm，2．7μm），以乙腈．0．1％甲酸水溶液为流动相梯度洗脱，分离苯乙双胍等25种化合物，在电喷雾离子化正离子或负离子模式下，以多反应监测方式（multiple reaction monitoring，MRM）检测。结果二甲双胍等3种化合物在进样浓度为50～1000pg／L范围内线性关系良好，妥拉磺脲等5种化合物在25～500μg／L范围内线性关系良好，其余20种化合物在5～100gg／L范围内线性关系良好，相关系数（r）均大于0．99。各化合物在定量限（1imit of quantity,LOQ）I倍、2倍、10倍添加水平下的平均加标回收率为48．6％～134．4％，相对标准偏差（relative standar ddeviation，RSD）为0．1％～8．4％（n=6）。二甲双胍等3种化合物的定量限为500μg／kg，妥拉磺脲等5种化合物的定量限为250μg／kg，苯乙双胍等20种化合物的定量限为50μg／kg。结论本方法灵敏、高效，可用于测定保健食品中降糖类非法添加化合物含量。 |
| Abstract_FL | Objective To establish an analytical method for the determination of 28 adulterated anti-diabetic compounds in health foodsby ultra performance liquid chromatography-triple quadrupole mass spectrometry. Methods A Merck SeQuant ZIC-HILIC column (100 mm×2.1 mm, 3.5 μm) was used with acetonitrile-0.1％ formic acid aqueous solution containing 10 mmol/L ammonium formate as mobile phases by gradient elution for separating 3 compounds such as metformin. A Waters CORTECS T3 column (100 mm×2.1 mm, 2.7 μm) was used with acetonitrile-0.1％formicacid aqueous solution as mobile phases by gradient elution for separating 25 compounds such as phenformin. The compounds were detected by electrospray ion souce in positive or negative mode with multiple reaction monitoring (MRM) mode.Results The calibration curves showed good linearities for 3 compounds such as metformin in the range of 50～1000μg/L, and for 5 compounds such as tolazamide in the range of 25～500μg/L, and for 20 compounds such as phenformin in the range of 5～100μg/L, respectively. The correlation coefficients (r) of the standard calibration curves for the 28 analytes were all above 0.99. The recoveries of the 28 compounds at spiked levels of limit of quantity (LOQ), double LOQ, 10 times of LOQ were in the range of 48.6％～134.4％, and the relative standard deviations (RSDs) were 0.1％～8.4％ (n=6). The LOQs were 500μg/kg for 3 compounds such as metformin, 250μg/kg for 5 compounds such as tolazamide, 50μg/kg for the other 20 compounds such as phenformin, respectively.Conclusion This method is selective, sensitive and accurate, which is suitable for detecting adulterated anti-diabetic compounds in health foods. |
| Author | 胡青;孙健;于泓;冯睿;张甦;张静娴;毛秀红;季申 |
| AuthorAffiliation | 上海市食品药品检验所,上海201203 |
| AuthorAffiliation_xml | – name: 上海市食品药品检验所,上海,201203 |
| Author_FL | HU Qing SUN Jian ZHANG Jing-Xian JI Shen ZHANG Su FENG Rui YU Hong MAO Xiu-Hong |
| Author_FL_xml | – sequence: 1 fullname: HU Qing – sequence: 2 fullname: SUN Jian – sequence: 3 fullname: YU Hong – sequence: 4 fullname: FENG Rui – sequence: 5 fullname: ZHANG Su – sequence: 6 fullname: ZHANG Jing-Xian – sequence: 7 fullname: MAO Xiu-Hong – sequence: 8 fullname: JI Shen |
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| Keywords | 保健食品 health foods ultra performance liquid chromatography-tandem mass spectrometry adulteration 非法添加 超高效液相色谱-三重四极杆质谱法 降糖 anti-diabetic |
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| Notes | Objective To establish an analytical method for the determination of 28 adulterated anti-diabetic compounds in health foods by ultra performance liquid chromatography-triple quadrupole mass spectrometry. Methods A Merck SeQuant ZIC-HILIC column （100 mm×2.1 mm, 3.5 μm） was used with acetonitrile-0.1% formic acid aqueous solution containing 10 mmol/L ammonium formate as mobile phases by gradient elution for separating 3 compounds such as metformin. A Waters CORTECS T3 column （100 mm×2.1 mm, 2.7 μm） was used with acetonitrile-0, l%formicacid aqueous solution as mobile phases by gradient elution for separating 25 compounds such as phenformin. The compounds were detected by electrospray ion souce in positive or negative mode with multiple reaction monitoring （MRM） mode. Results The calibration curves showed good linearities for 3 compounds such as metformin in the range of 50-1000 ~tg/L, and for 5 compounds such as tolazamide in the range of 25-500 pg/L, and for 20 compounds such as phenformin in the range of 5-10 |
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| PublicationTitle | 食品安全质量检测学报 |
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| SubjectTerms | 保健食品 超高效液相色谱-三重四极杆质谱法 降糖 非法添加 |
| Title | 超高效液相色谱-三重四极杆质谱法测定保健食品中28种降糖类非法添加化合物 |
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