高效液相色谱-串联质谱法测定动物源性食品中矮壮素残留

建立了高效液相色谱-串联质谱测定动物源性食品中矮壮素残留的分析方法。样品经含1%（v/v）乙酸的乙腈溶液提取、正己烷脱脂、阳离子固相萃取柱（PCX）净化，采用Venusil MP C18（2）色谱柱（150 mm×2.1 mm，3 μm）分离，以乙腈和0.1%（v/v）甲酸水溶液为流动相进行梯度洗脱，采用电喷雾电离、正离子模式扫描，多反应监测模式（MRM）检测，基质匹配标准曲线内标法定量。结果表明：矮壮素在0.200~500 μg/L范围内呈良好线性，相关系数（r²）均不低于0.9993，方法的定量限为0.500 μg/kg；以猪肉、牛肉、羊肉、鸡肉、鸡蛋、猪肾、牛肝、羊肾、鸡肝、牛奶为基质，矮壮素的平均加标回收率为93.4%~101%，相对标准偏差为2.3%~8.0%。该方法基质干扰小，灵敏度高，准确可靠，适用于动物源性食品中矮壮素残留的定量检测。

Determination of chlormequat chloride residues in animal derived foods by high performance liquid chromatography-tandem mass spectrometry

A method for the determination of chlormequat chloride (CCC) residues in animal derived foods by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was developed. The samples were extracted with acetonitrile containing 1% (v/v) acetic acid and defatted with n-hexane, followed by clean-up on a cationic solid phase extraction column. The analytes were separated on a Venusil MP C18(2) column (150 mm×2.1 mm, 3 μm) under a gradient elution program using acetonitrile and 0.1% (v/v) formic acid aqueous solution as the mobile phases. Then, the analytes were detected by tandem mass spectrometry using a positive electrospray ionization (ESI⁺) source in the multiple reaction monitoring (MRM) mode. Matrix-matched internal standard calibration curves were used for quantitative analysis. The calibration curves showed good linearity in the range of 0.200-500 μg/L for CCC, with correlation coefficients (r²) no less than 0.9993. The limit of quantification (LOQ) of the method was 0.500 μg/kg. The average recoveries of CCC in pork, beef, mutton, chicken, egg, pig kidney, beef liver, sheep kidney, chicken liver and milk matrices at spiked levels of 0.500-500 μg/kg were 93.4%-101%, and the relative standard deviations were 2.3%-8.0%. The method has less matrix interference, with high sensitivity, accuracy and reliability, and it is suitable for the quantitative detection of CCC residues in animal derived foods.