亲水作用色谱-串联质谱测定尿液中尼古丁和可替宁

发布时间：2018-04-05 15:23

本文选题：亲水作用色谱-串联质谱　切入点：同位素稀释　出处：《色谱》2017年08期

【摘要】：建立了测定人尿液中尼古丁和可替宁含量的亲水作用色谱-串联质谱(HILIC-MS/MS)方法。尿样加入尼古丁-d4和可替宁-d3同位素内标后,用水稀释10倍,经过滤后的滤液由超高效液相色谱-串联质谱(UPLC-MS/MS)进行分离分析。采用ACQUITY UPLC~汶BEH HILIC色谱柱(50 mm×3.0 mm,1.7μm),以甲醇和体积分数为0.1%的氨水为流动相,流速为0.2 mL/min,在电喷雾电离源正离子模式下测定尿液中尼古丁和可替宁的含量,用标准曲线法定量。尼古丁和可替宁在1.0~1 000μg/L范围内线性关系良好,相关系数分别为0.994 9和0.995 8;检出限分别为0.082μg/L和0.077μg/L;定量限分别为0.27μg/L和0.26μg/L;加标回收率分别为90.4%~103.5%和93.0%~104.6%;相对标准偏差分别为4.80%~6.21%和4.22%~7.15%。应用所建立的方法测定了200份尿样,结果表明,吸烟人群尿中尼古丁含量为26.68~854.30μg/L,可替宁含量为36.66~1 191.18μg/L(n=86,M_(nicotine)=76.00μg/L,M_(nicotine)=83.52μg/L,M为中位数);非吸烟人群尿中尼古丁含量为5.08~69.66μg/L,可替宁含量为3.16~28.21μg/L(n=114,Mnicotine=7.53μg/L,M_(nicotine)=3.79μg/L)。该方法快速灵敏,操作简单,适用于尿样中尼古丁和可替宁的批量测定,能满足烟草暴露评价的需要。
[Abstract]:A hydrophilic interaction chromatography determination of nicotine and cotinine in human urine by tandem mass spectrometry (HILIC-MS/MS) method. Adding -d4 and -d3 urine nicotine cotinine isotope internal standard and diluted 10 times after filtration filtrate by ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) was isolated by ACQUITY UPLC~ Wen analysis. BEH HILIC column (50 mm * 3 mm, 1.7 m), with 0.1% volume fraction of methanol and ammonia water as mobile phase, the flow rate is 0.2 mL/min, determination of nicotine and cotinine in urine in the electrospray ionization source in positive ion mode, using the quantitative standard curve method. The nicotine and cotinine in 1.0~1 000 g/L good linear range, the correlation coefficients were 0.9949 and 0.9958 respectively; the detection limit was 0.082 g/L and 0.077 g/L; the limit of quantitation were 0.27 g/L and 0.26 g/L; the recovery rate was 90.4%~103.5% and 93 respectively. %~104.6%; the relative standard deviations were 4.80%~6.21% and 4.22%~7.15%. using the 200 urine samples, the results showed that smoking nicotine content in urine was 26.68~854.30 g/L, 36.66~1 191.18 g/L for cotinine (n=86, M_ (nicotine) =76.00 g /L M_ (nicotine) =83.52 g/L, M the median non smoking population); nicotine content in urine was 5.08~69.66 g/L, 3.16~28.21 g/L for cotinine (n=114, Mnicotine=7.53 g/L, M_ (nicotine) =3.79 g/L). This method is simple, rapid and sensitive, suitable for batch determination of nicotine and cotinine in urine, can satisfy the need of tobacco exposure assessment.

【作者单位】：四川大学华西公共卫生学院卫生检验与检疫系;四川省疾病预防控制中心;
【基金】：四川大学国际合作评估吸烟者牙种植体存活率的前瞻性、非随机化临床研究资助项目~~
【分类号】：O657.63;R446.12

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