本文選題：親水作用色譜-串聯(lián)質(zhì)譜　切入點(diǎn)：同位素稀釋　出處：《色譜》2017年08期

【摘要】：建立了測(cè)定人尿液中尼古丁和可替寧含量的親水作用色譜-串聯(lián)質(zhì)譜(HILIC-MS/MS)方法。尿樣加入尼古丁-d4和可替寧-d3同位素內(nèi)標(biāo)后,用水稀釋10倍,經(jīng)過濾后的濾液由超高效液相色譜-串聯(lián)質(zhì)譜(UPLC-MS/MS)進(jìn)行分離分析。采用ACQUITY UPLC~汶BEH HILIC色譜柱(50 mm×3.0 mm,1.7μm),以甲醇和體積分?jǐn)?shù)為0.1%的氨水為流動(dòng)相,流速為0.2 mL/min,在電噴霧電離源正離子模式下測(cè)定尿液中尼古丁和可替寧的含量,用標(biāo)準(zhǔn)曲線法定量。尼古丁和可替寧在1.0~1 000μg/L范圍內(nèi)線性關(guān)系良好,相關(guān)系數(shù)分別為0.994 9和0.995 8;檢出限分別為0.082μg/L和0.077μg/L;定量限分別為0.27μg/L和0.26μg/L;加標(biāo)回收率分別為90.4%~103.5%和93.0%~104.6%;相對(duì)標(biāo)準(zhǔn)偏差分別為4.80%~6.21%和4.22%~7.15%。應(yīng)用所建立的方法測(cè)定了200份尿樣,結(jié)果表明,吸煙人群尿中尼古丁含量為26.68~854.30μg/L,可替寧含量為36.66~1 191.18μg/L(n=86,M_(nicotine)=76.00μg/L,M_(nicotine)=83.52μg/L,M為中位數(shù));非吸煙人群尿中尼古丁含量為5.08~69.66μg/L,可替寧含量為3.16~28.21μg/L(n=114,Mnicotine=7.53μg/L,M_(nicotine)=3.79μg/L)。該方法快速靈敏,操作簡(jiǎn)單,適用于尿樣中尼古丁和可替寧的批量測(cè)定,能滿足煙草暴露評(píng)價(jià)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.

【作者單位】： 四川大學(xué)華西公共衛(wèi)生學(xué)院衛(wèi)生檢驗(yàn)與檢疫系;四川省疾病預(yù)防控制中心;
【基金】：四川大學(xué)國(guó)際合作評(píng)估吸煙者牙種植體存活率的前瞻性、非隨機(jī)化臨床研究資助項(xiàng)目~~
【分類號(hào)】：O657.63;R446.12

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