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1 5 5 Vol. 5 No Journal of Food Safety and Quality May., ,2-1,3- 高家敏, 黄湘鹭, 宋钰, 曹进 *, 张庆生 (, ) 摘要 : 目的 1,2-1,3- 方法, 结果 1,2-1,3-3.03~ mg/l 3.06~ mg/l, , 0.95 mg/kg 0.96 mg/kg (S/N=3), mg/kg 3, 1,2-1,3-93.7%~107.8%, RSD 0.97%~2.26% (n=9) 结论, 1,2-1,3-, 关键词 : ; 1,2-; 1,3-; Measurement of 1,2 propanediol and 1,3 propanediol in salad by gas chromatography GAO Jia-Min, HUANG Xiang-Lu, SONG Yu, CAO Jin *, ZHANG Qing-Sheng (National Institutes for Food and Drug Control, Beijing , China) ABSTRACT: Objective To establish a method of simultaneous determination of 1,2 propanediol and 1,3 propanediol in salad by gas chromatography. Methods Propanediols in samples were extracted with anhydrous alcohol concentrated by rotary evaporator and analyzed by gas chromatography. Results The method showed a good linearity over the range of 3.03~ mg/l for 1,2 propanediol and 3.06~ mg/l for 1,3 propanediol, with correlation coefficients of and 1 respectively. The limits of detection for 1,2 propanediol and 1,3 propanediol were 0.95 mg/kg and 0.96 mg/kg (S/N=3), respectively. The recoveries were 93.7%~107.8% at the spiked level of 60, 30, 3 mg/kg with the RSD between 0.97% and 2.26% (n=9). Conclusion This method is sensitive, reliable, and simple, which has been applied for the determination of 1,2 propanediol and 1,3 propanediol in salad with satisfactory results. KEY WORDS: salad; 1,2 propanediol; 1,3 propanediol; gas chromatography 1 引言 1,2-1,3-,,,,, [1-3],, * 通讯作者 :,, cao1208@gmail.com *Corresponding author: CAO Jin, Associate Research, National Institutes for Food and Drug Control, No.2, Tiantan Xili, Dongcheng District, Beijing, China. cao1208@gmail.com

2 5, : 1,2-1,3-1513,,,,, ; [4,5],,, (GB ) [6], 3.0 g/kg; (), 1.5 g/kg, 1, 2- (GB/T ) [7] 1,2-, 210 nm,,, [8,9] (fourier transform infrared spectroscopy, FTIR) [10], ( ) (2010 ) [11] 1,2-1,2- [12-19], [20],, 1,2-1,3-,,,,, 1,2-1,3-, 0.95 mg/kg 0.96 mg/kg, 2 材料与方法 2.1 仪器与试剂 7890A (flame ionization detector, FID), ; DB-WAX (30 m 0.25 mm, 0.25 µm), ; SGHK-500, ; R-210, BUCHI ; Vortex-Genie 2, Scientific Industries ; Micro 21R, Thermo ; AL204, Mettler Toledo ; 600A, ; KQ3200DE,, TEDIA ;, 1,2-99.5%, 1,3-98%, Sigma : 2.2 色谱条件 : 230 ; : 80, 3 min, 2 /min 110, 10 min, 2 /min 130, 10 /min 220, 5 min; 250, N 2, 1.0 ml/min, 30 ml/min, 300 ml/min, (N 2 ) 40 ml/min, 2:1, 1 μl 2.3 1,2- 丙二醇和 1,3- 丙二醇混合标准工作溶液的制备 1,2-1,3-1 g( g), 100 ml, 10 mg/ml 1,2-1, ml 100 ml,,, 1,2-1, mg/l 2.4 样品处理 5 g 50 ml, 20 ml,

3 min, 10 min, r/min 5 min, 2 10 ml,,, 5 ml 1.5 ml 2 ml, 0.1 g, 2 min, r/min 5 min, 2.5 样品测定 1 μl 1,2-1,3-,, 2.6 1,2- 丙二醇和 1,3- 丙二醇含量计算 V 1000 X = c 1000 m 1000 : X 1,2-1,3-, g/kg; c 1,2-1,3-, μg/ml; V, ml; m, g 2 Fig. 2 Chromatogram of the meat blank samples 3 结果与分析 3.1 方法的选择性 1,2-1,3-,, ( 1~5), 1,2-1,3- Fig. 3 3 Chromatogram of 1,2 propanediol and 1,3 propanediol standards in the meat blank samples : 1 1,2-, 2 1,3- Peak1 1,2 propanediol, Peak2 1,3 propanediol 1 1,2-1,3- Fig. 1 Chromatogram of standard solution of 1,2 propanediol and 1,3 propanediol : 1 1,2-, 2 1,3- Peak1 1,2 propanediol, Peak2 1,3 propanediol Fig. 4 4 Chromatogram of the vegetable blank sample

4 5, : 1,2-1, Supelco ENVI-Carb Waters Oasis Wax, -N- (primary secondary amine, PSA, 40~70 µm) C 18,, 1,2-1,3-, 5 Fig. 5 Chromatogram of 1,2 propanediol and 1,3 propanediol standards in the vegetable blank samples : 1 1,2-, 2 1,3- Peak1 1,2 propanediol, Peak2 1,3 propanediol 3.2 前处理方法的选择 :,,,, 30%,,,,,,,,,, 1, 2- (GB/T ) [7],,,,, 3.3 线性范围检出限和定量限 1,2-1,3-,, 100 mg/l 50 μl 150 μl,, 3 10, 1,2-1,3- (S/N=3) (S/N=10), 重复性精密度和稳定性 5 g 18, ( mg/kg)3 1,2-1,3- ( 100 mg/l 150 μl; 500 mg/l 300 μl; 500 mg/l 600 μl, 6,,,, RSD 0.76%~1.39%, 1 6,,, RSD 0.87%~1.66%, h,,, RSD 0.87%~1.66%, 2 Table 1 表 1 线性范围线性方程相关系数检出限 (LOD) 和定量限 (LOQ) Linear ranges,regression equations, correlation coefficients, limits of determination and limits of quantification (mg/l) (r) (mg/kg) (mg/kg) 1, Y=2.6716X , Y=2.7457X

5 Table 2 表 2 1,2- 丙二醇和 1,3- 丙二醇的重复性精密度和稳定性 Repeatability, precision and stability of 1,2 propanediol and 1,3 propanediol (mg/kg) (mg/kg) RSD(%) (mg/kg) RSD(%) 0 h 2 h 4 h 8 h 12 h 24h RSD(%) , , Table 3 表 3 不同添加水平下 1,2- 丙二醇和 1,3- 丙二醇的加标回收率 Average spike recoveries of 1,2 propanediol and 1,3 propanediol at different fortification levels (mg/kg) (%) RSD(%) , , 回收率 5 g 9, 3 1,2-1,3-, 3, 3,,, 3, mg/kg 3, 1,2-1,3-93.7%~107.8%, RSD 0.97%~2.26%, 3.6 样品测定, 42, 6,,, 6, 1,2-1,3-, 67.4 mg/kg 48.3 mg/kg 4 结论 1,2-1,3-, 1,2-1,3-1,2-1,3-3.03~ mg/l 3.06~ mg/l, mg/kg mg/kg 3, 1,2-1,3-93.7%~107.8%,

6 5, : 1,2-1, ,2-1,3- Fig. 6 Determination results of 1,2 propanediol and 1,3 propanediol in salad samples(n=42) (No.)1~14, 15~38, 39, 40~42 参考文献 [1]. 枓 [M]. :, Yao J. Application directory of pharmaceutical excipients [M]. Beijing: Medicine Science and Technology Press of China, [2]. [M]. :, Yang YH. Food additives technique [M]. Beijing: China Quality Press, Standards press of China, [3],,,. [J]., 2013, 175(6): Lan YZ, Zhang JS, Peng Z, et al. The impact and application of propylene glycol added to cellulose acetate cigarette filter [J]. Light Ind Sci Technol, 2013, 175(6): [4]. [M]. :, Liu C. Practical of food additives [M]. Beijing: Beijing University of Technology press, [5]. [M]. :, Ling GT. Handbook of food additives [M]. Beijing: Chemical Industry Press, [6] GB [S]. GB National Food Safety Standards-Standards for uses of food additives [S]. [7] GB/T ,2-[S]. GB/T Determination of 1,2-propanediol in Foods [S]. [8],,,. [J]., 2002, 30(6): Li Z, Yang GY, Huang HT, et al. Determination of sugars, glycerol and propylene glycol with high performance liquid chromatography in tobacco sauce [J]. Chin J Anal Chem, 2002, 30(6): [9],,,. [J]. :, 2006, 42(12): Chen ZY, Xu RF, Miu MM, et al. Determination of some moisturizing ingredients in tobacco feed liquid by high performance liquid chromatography [J]. Phys Test Chem Anal:Chem Anal, 2006, 42(12): [10],,,. [J]., 2002, 19(4): Li ZJ, Zhong ZG, Li HS, et al. Direct determination of the content of propanediol by FTIR [J]. Chin J Spectrosc Lab, 2002, 19(4): [11]. [M]. :, State Pharmacopoeia Committee. Pharmacopeia of the People's Republic of China [M]. Beijing: Chianese Medical Science And

7 Technology Press, [12],,,. [J]., 2010, 31(10): ,181. Lv Q, Zuo Y, Mai CH, et al. Measurement of propanediols in food by gas chromatography [J]. Food Res Dev, 2010, 31(10): ,181. [13],,,. [J]., 2013, 33(10): Ma MX, Fu R, Guo HW, et al. GC determination of propylene glycol in rifamycin sodium injection [J]. Chin J Pharm Anal, 2013, 33(10): [14],,,. K1 1,2-[J]., 2013, 11(9): Li L, Liu YM, Long HY, et al. Determination of 1,2-propylene glycol in Vitamin K1 injection by GC [J]. Cent South Pharm, 2013, 11(9): [15],. GC [J]., 2008, 22(6): Li WL, Qiu J. Determination of propylene glycol and diethylene glycol in puerarin injection by GC [J]. Chin Pharm Aff, 2008, 22(6): [16],,,. GC/MS 1,2[J]., 2011, 284: Zhang J, Li P, Sun SH, et al. Simultaneous determination of 1,2-propylene glycol,glycerol and triethylene glycol in smokeless tobacco products by gas chromatography-mass spectrometry [J]. Tob Sci Technol, 2011, 284: [17],,,. GC-MS [J]., 2008, 28(6): Jin PF, He XR, Zou D, et al. Quality control and diethylene glycol test of propylene glycol by GC-MS [J]. Chin J Pharm Anal, 2008, 28(6): [18],,,. [J]., 2011, 12: Chen Z, Li JX, Li ZX, et al. Determination of reaction products for hydrogenolysis of glycerol to propanediols by gas chromatography [J]. Chem World, 2011, 12: [19] 琲. 1,3- [J]., 2005, 12:81 Wang B. Quantity analysis of 1,3-propanediol by gas chromatography [J]. China Sci Technol Inf, 2005, 12:81. [20]? [EB/OL] ng-in-your-salad-dressing/ What the heck is this doing in your salad dressing? [EB/OL] ng-in-your-salad-dressing/ 作者简介 ( 责任编辑 : 邓伟 ) 高家敏, 主管药师, 主要研究方向为药物分析 gaojiamin@nifdc.org.cn 曹进, 副研究员, 博士, 主要研究方向为分析化学 cao1208@gmail.com

g ml 10% ph 色谱条件 kinetex C μm 100 A 4. 6 mm 150 mm 25 5 μl A B 10 mmol /L ml /min

g ml 10% ph 色谱条件 kinetex C μm 100 A 4. 6 mm 150 mm 25 5 μl A B 10 mmol /L ml /min 25 4 2013 8 监测技术 5 1 2 1 ( 1. 江苏省疾病预防控制中心, 江苏南京 210009; 2. 南京医科大学第二附属医院, 江苏南京 210029) 5 Phenomenex kinetex C 18 2. 6 μm 4. 6 mm 150 mm 10 mmol /L ph 2. 5 + 60 40 DAD 280 nm 5 20. 0 mg /L ~ 100 mg /L 0.