UPLC-MS/MS法测定"红牛"饮料中盐酸可卡因的含量

目的: 建立测定"红牛"饮料中非法添加的盐酸可卡因的含量的超高压液相色谱-质谱联用方法。 方法: 选用ACQUITYUPLC^RBEH C₁₈(1.7 μm,2.1 mm×100 mm)色谱柱,以甲醇-醋酸铵溶液(取醋酸铵1.5 g、甲酸1 mL,用水1000 mL制得)(30∶ 70,v/v)为流动相,流速为0.2 mL·min^-1,检测波长为233 nm。样品经固相萃取柱进行富集,再洗脱及定容处理后进样,柱温:室温,进样量:10 μL。选用Waters Qattro micro^TM API型三重四极杆串联质谱仪的多重反应监测(MRM)及子离子扫描(Daughter scan)方式进行检测。 结果: 盐酸可卡因浓度在2.16~5408 ng·mL^-1范围,其浓度与定量离子对的峰面积呈良好的线性关系,r=0.9999,检测限为0.216 ng·mL^-1。精密度RSD为1.4%(n=6),回收率为98.9%(RSD=1.1%,n=9),稳定性好。 结论: 建立的UPLC-MS/MS方法灵敏度高,回收率及重现性好,可检出相当于每升"红牛"饮料中10.8 ng盐酸可卡因。

Objective: To develop an UPLC-MS/MS method for the determination of cocaine hydrochloride residues in " Redbull" drink. Method: Cocaine hydrochloride was extracted from the "Redbull" with solid-phase extraction,and then separated on a ACQUITYUPLC^R BEH C₁₈(1.7 μm,2.1 mm×100 mm)column,the mobile phase consisted of methanol-ammonium acetate solution(dissolve 1.50 g of ammonium acetate and 1.0 mL of formic acid and dilute to 1000 mL with water)(30∶ 70,v/v),the flow rate was 0.2 mL·min^-1,the detection wavelength was at 233 nm,the column temperature was room temperature and the injection volume was 10 μL.Detection was carried out by multiple reaction monitoring and Daughter scan on Qattro micro^TM API UPLC-MS/MS system. Results: The calibration cure was linear in the of range 2.16-5408 ng·mL^-1(r=0.9999).Limit of detection was 0.216 ng·mL^-1.The relative deviation of precision was 1.4%(n=6).The recovery of cocaine hydrochloride was 98.9%(RSD=1.1%,n=9) and stability was good. Conclusion: It is a sensitive,reliable method for the determination of cocaine hydrochloride residues in "Redbull".It can dectecte 10.8 ng of cocaine hydrochloride residues in 1 L of "Redbull" drink.