作者：严拯宇¹, 牛倩倩¹, 牟明瑶¹, 刘廷生², 曹志然², 廖声华¹

作者单位：1. 中国药科大学理学院, 江苏 南京 211198;
2. 中国药科大学生命科学与技术学院, 江苏 南京 211198

关键词：毛细管气相色谱法;N-亚硝胺;迁移量;水杯垫圈

摘要：

建立毛细管气相色谱法用于测定水杯密封垫圈中5种N-亚硝胺的迁移量。采用DB-5（30 m0.53 mm，1.00 m）毛细管柱；程序升温：38℃保持4 min，以15℃/min的速率升至250℃保持4 min；N2为载气，流量为4.0 mL/min；氢火焰离子化检测器（FID），检测器温度为250℃；进样口温度为280℃；进样量为1.0 L。以2-叔丁基对甲酚为内标，通过内标对比法计算样品中5种N-亚硝胺的迁移量。在该色谱条件下，N-亚硝基二甲胺、N-亚硝基二乙胺、N-亚硝基吗啉、N-亚硝基哌啶和N-亚硝基二丁胺之间均能完全分离。此5种N-亚硝胺化合物分别在0.01～0.50，0.10～0.75，0.02～0.75，0.02～0.75，0.01～0.50 mg/kg的质量浓度范围内线性关系良好（r2=0.991 6～0.995 5）；进样精密度（RSD）均小于5.0%（n=6）；平均回收率为88.9%～96.7%（RSD5.0%，n=9）。定量限分别为0.01，0.10，0.02，0.02，0.01 mg/kg（信噪比为10∶1）；检测限分别为2.0，20，2.0，2.0，2.0 g/kg（信噪比为3∶1）。采用本法测定3个厂家各2批水杯垫圈中N-亚硝胺的迁移量，均低于规定限度。该方法简便、准确、灵敏、重复性好、成本低，可用于水杯垫圈中N-亚硝胺迁移量的检测。

Determination of migration levels of N-nitrosamines in cup gasket by capillary GC

YAN Zhengyu¹, NIU Qianqian¹, MOU Mingyao¹, LIU Tingsheng², CAO Zhiran², LIAO Shenghua¹

1. School of Science, China Pharmaceutical University, Nanjing 211198, China;
2. School of Life Science and Technology, China Pharmaceutical University, Nanjing 211198, China

Abstract: To establish a capillary GC method for simultaneous determination of migration levels of 5 N-nitrosamines in cup gasket. Methods DB-5 capillary column(30 m×0.53 mm,1.00 μm) was selected as chromatographic column, the initial temperature of which was 38℃ for 4 min and gradually reached to 250℃ for 4 min with the rate of 15℃/min. Nitrogen was selected as carrier gas at a flow rate of 4.0 mL/min and FID was used to detect N-nitrosamines at 250℃. The temperature of injection chamber was set at 280℃ and the volume of injection was 1.0 μL. 2-tert-butyl-p-cresol was used as internal standard compound, five kinds of component in the samples were calculated by internal standard comparison method. N-nitrosodimethylamine, N-nitrosodiethylamine, N-nitrosomorpholine, N-nitrosopiperidine and N-nitrosodi-n-butylamine were completely separated under the established chromatographic condition. Good linear relationship were obtained for these five N-nitrosamines in the range of 0.01-0.50, 0.10-0.75, 0.02-0.75, 0.02-0.75, 0.01-0.50 mg/kg, respectively. The correlation coefficients of these five kinds of N-nitrosamines were ranged from 0.991 6 to 0.995 5. The relative standard deviation of sampling precisions were less than 5.0%(n=6) and the average recovery were ranged from 88.9% to 96.7%(RSD<5.0%, n=9). The limits of quantification for them were 0.01, 0.10, 0.02, 0.02 and 0.01 mg/kg respectively(S/N=10:1). The limits of detection for them were 2.0, 20, 2.0, 2.0 and 2.0 μg/kg respectively (S/N=3:1). The migration levels of these five kinds of N-nitrosamines in the samples were lower than the limit of regulation in the samples. The method is simple, accurate, sensitive, repeatable and low cost. It is suitable for the determination of the migration levels of 5 N-nitrosamines in cup gasket.

Keywords: capillary GC;N-nitrosamines;migration level;cup gasket

2017, 43(1): 37-41  收稿日期: 2016-05-20;收到修改稿日期: 2016-07-19

基金项目: 大学生创新药物研制能力提高项目（J1030830）国家级大学生创新创业训练计划项目（G15019）

作者简介: 严拯宇(1955-),女,河南开封市人,教授,博士生导师,主要从事仪器分析、药物分析方面的研究。

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