液相色谱-串联质谱法测定畜禽肌肉和表皮组织中松香酸、脱氢松香酸和胡椒酸
目的 建立液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometry, LC-MS/MS)测定畜禽肌肉和表皮组织中松香酸、脱氢松香酸和胡椒酸的分析方法。方法 均质样品中加入乙腈提取目标物, 经涡旋分散、振荡提取、离心和固相萃取柱净化。提取液以乙酸铵-甲醇为流动相梯度洗脱C18色谱柱分离, 5 mmol的乙酸铵水溶液和甲醇为流动相进行梯度洗脱, 三重四极杆质谱ESI+/ESI-切换模式检测, 以特征离子峰和保留时间定性, 定量离子峰面积定量。结果 松香酸、脱氢松香酸和松香酸的检出限(limits of detection, LOD)分别为0.36、0.87和1.40 μg/kg, 定量限(limits of quantification, LOQ)为1.08、2.61、4.20 μg/kg。松香酸、脱氢松香酸线性浓度范围为5.0?200.0 μg/kg, 松香酸线性浓度范围为20.0?500.0 μg/kg, 相关系数(r)在0.999以上。分别添加定量限1、2、4倍的浓度验证加标回收率, 3个浓度水平的回收率为68.5%~107.6%, 相对标准偏差为5.3%~12.6%(n=6)。结论 该方法快速、准确、灵敏, 适用于监管部门对市售畜禽食品中工业松香残留的检测。
Objective To establish a method for the determination of abietic acid, dehydroabietic acid and piperic acid in livestock and poultry by liquid chromatography-tandem mass spectrometric (LC-MS/MS). Methods Samples were extracted with acetonitrile and water solution, which were purified by vortex dispersion, concussion extraction, centrifugation and solid phase extraction column purification. And then the abieticacid, dehydroabietic acid and piperic acid in the extracts were separated on C18 using a gradient elution program with 5mmol ammonium acetate in water (A) and methanol(B) as mobile phase. Using LC–MS/MS (ESI+/ESI-) with multiple reactions monitoring (MRM), identification of the major components of the abietic acid, dehydroabietic acid and piperic acid were performed based upon ion peak and retention time. Quantitative analysis was based on ion peak area. Results The limits of detection (LOD) for the abietic acid, dehydbitic acid and piperic acid were 0.36, 0.87 and 1.40 μg/kg, respectively, and limits of quantification (LOQ) were 1.08, 2.61, and 4.20 μg/kg. The linear concentrations of abietic acid, dehydbitic acid were in the range of 5.0?200.0 μg/kg and the linear concentration of piperic acid was 20.0?500.0 μg/kg, and the correlation coefficients were greater than 0.999. The recoveries were ranged from 68.5%?107.6% for the 3 targets with 3 spiked levels of 1, 2, 4 times of quantiative limits. The relative standard deviations (RSDs) were 5.3%?12.6% (n=6). Conclusion The proposed method is fast, accurate and sensitive, which is suitable for the detection of industrial rosin residues in livestock and poultry food sold on the market by regulatory authorities.
标题：液相色谱-串联质谱法测定畜禽肌肉和表皮组织中松香酸、脱氢松香酸和胡椒酸
英文标题：Simultaneous determination of abietic acid, dehydroabietic acid and pipericacid in muscle and skin tissue of livestock and poultry by liquid chromatography-tandem mass spectrometry
作者：
张毅 深圳市检验检疫科学研究院
罗耀 深圳市检验检疫科学研究院
温景岚 深圳市检验检疫科学研究院
中文关键词:松香酸,脱氢松香酸,胡椒酸,液相色谱-串联质谱法,畜禽肌肉,表皮组织,
英文关键词:abietic acid,dehydroabietic acid,piperic acid,liquid chromatography tandem mass spectrometry,animal muscle,epidermal tissue,
发表日期：2020-07-20
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