7 8 Vol. 7 No. 8 2016 8 Journal of Food Safety and Quality Aug., 2016 * 梁国华 (, 536000) 摘要 : 目的 (high performance liquid chromatography, HPLC) 方法 10%, 30 min, - (35:65, V:V), 1.0 ml/min, Shimadzu VP-ODS (250 mm 4.6 mm, 5 μm), 290 nm HPLC, 结果 0.0216~0.216 μg/ml, 0.99998, 98.1%, 1.63%, 0.1 μg/ml 结论, 关键词 : ; ; Determination of cinnamaldehyde in Chinese Jing Wine by high performance liquid chromatography LIANG Guo-Hua * (Guangxi Beihai Institute for food and Drug Control, Beihai 536000, China) ABSTRACT: Objective To establish a method for the determination of cinnamaldehyde in Chinese Jing Wine by high performance liquid chromatography (HPLC). Methods Samples were extracted with 10% methanol by ultrasonic for 30 min, and separated by a Shimadzu VP-ODS column (250 mm 4.6 mm, 5 μm) with acetonitrile-water (35:65, V:V) as mobile phase at the flow rate of 1.0 ml/min. Then the samples were detected by HPLC at the detection wavelength of 290 nm. Meanwhile, the mobile phase ratio and extractant were optimized. Results The cinnamaldehyde had a good linearity relationship at the range of 0.0216~0.216 μg/ml, and the correlation coefficient was 0.99998. The average recovery was 98.1%, the relative standard deviation was 1.63%, and the detection limit was 0.1 μg/ml. Conclusion The method is rapid, accurate and reproducible, which can be used for the determination of cinnamaldehyde in Chinese Jing Wine. KEY WORDS: Chinese Jing Wine; cinnamaldehyde; high performance liquid chromatography 1 引言, [1],,, [2] (high performance liquid chromatography, HPLC),,, * 通讯作者 :,, E-mail: lgh1280@sina.com *Corresponding author: LIANG Guo-Hua, Associate Chief Pharmacist, Guangxi Beihai Institute for Food and Drug Control, Beihai 536000, China. E-mail: lgh1280@sina.com
3104 7 2 材料与方法 2.1 仪器 LC-2010AHT ( VWD, ); XA205DU ( - ) 2.2 试剂, 111710-200513, ( ), (, ), 2.3 实验方法 2.3.1 色谱条件 : Shimadzu VP-ODS(250 mm 4.6 mm, 5 μm), ; : - (35:65, V:V); : 290 nm : 35 ; : 1.0 ml/min; : 10 μl; 3000 2.3.2 对照品溶液的制备 10.80 mg, 50 ml, ; 1 ml 100 ml, 35%, ( 2.16 μg/ml) 2.3.3 供试品溶液的制备 1 g 10 ml, 10%, 30 s, 0.22 μm, 2.3.4 空白对照溶液的制备,,, 2.3.3, 3 结果与分析 3.1 高效液相色谱流动相的选择 [3-22], - -0.085% -, - (35:65, V:V) -0.085% (25:75, V:V), -,, 20 min,, - (35:65, V:V) 3.2 样品提取溶剂浓度的选择 35% 25% 20% 15% 10% 5,, 10%, 3.3 方法学考察 3.3.1 专属性实验,, 1~ 3 1 Fig. 1 Chromatogram of reference substance
8 : 3105 2 Fig. 2 Chromatogram of sample 3 Fig. 3 Chromatogram of negative sample 3.3.2 线性范围 方法检出限 (2.16 μg/ml)0.1 0.3 0.5 0.7 1.0 ml 10 ml, 10%, 30 s, 0.22 μm, 2.3.1, X(μg/mL), Y(A), 0.0216~0.216 μg/ml, : Y=84111.16803X+59.73361(r=0.99998), 2.3.3, 2.3.1, 3, 0.1 μg/ml 3.3.3 精密度实验 10 μl, 6,,, (relative standard deviation, RSD) 0.528% 3.3.4 稳定性实验, 2.3.1 0 4 8 12 16 20 24 h 10 μl,, RSD 0.701%, 24 h 3.3.5 重复性实验, 6 (n=6), 2.3.3
3106 7 表 1 回收率结果 (n=9) Table 1 Results of recoveries (n=9) (ml) (μg) (μg) (μg) (%) (%) RSD(%) 0.5 0.254 0.648 0.8786 96.4 0.5 0.254 0.648 0.8985 99.5 0.5 0.254 0.648 0.8971 99.2 98.1 1.63 0.5 0.254 1.080 1.2925 96.2 0.5 0.254 1.080 1.3031 97.1 0.5 0.254 1.080 1.3285 99.5 0.5 0.254 2.160 2.3306 96.1 98.1 0.5 0.254 2.160 2.4005 99.4 0.5 0.254 2.160 2.4050 99.6 表 2 桂皮醛测定结果 (n=3) Table 2 Results of cinnamaldehyde (n=3) (μg/ml) (μg/ml) RSD(%) A 0.4155 B 0.4118 0.4314 1.33 C 0.4670, 2.3.1, 0.4607 μg/ml, RSD 0.584%, 3.3.6 加样回收率试验 9 ( 1~ 1 ), 0.5 ml, : 1~ 1 0.3 ml 4~ 4 0.5 ml 7~ 1 1.0 ml, 2.3.3, 2.3.1, RSD, 1 98.1%, RSD 1.63%, 3.4 样品测定 3, 2.3.3, 2.3.1, 2 4 结论, 参考文献 [1]. ( ) [S]. Pharmacopoeia commission of the ministry of public health of the people's Republic of China. Drug standards of the ministry of health of the people's Republic of China(Chinese medicinal preparation)eleventh volumes [S]. [2]. [M]. :, 1991. Luo HS. Advances in pharmacology and clinical research of traditional Chinese medicine [M]. Guangzhou: South China University of Technology Press, 1991. [3],,. HPLC [J]., 2012, 24(4): 54 56. Cai SH, Wen YG, Mo YQ. Determination of cinnamaldehyde in Jiawei Lingguishugan decoction by HPLC [J]. Strait Pharm J, 2012, 24(4): 54 56. [4],,,. HPLC [J]., 2013, 34(2): 230 232. An Y, Zhang XX, Liang JR, et al. Content determination of cinnamaldehyde in Disinfectant of Ruikeweirui by HPLC [J]. Shaanxi J Tradit Chin Med, 2013, 34(2): 230 232. [5],,,. 4 [J]. -, 2013, 15(2): 254 259. Hou XY, Wu C, Zhou YT, et al. Study on the content and distribution of 4 active components in different parts of cinnamon [J]. World Sci Technol Mod Tradit Chin Med, 2013, 15(2): 254 259. [6],. [J]., 2007, 16(4): 35 37. Lei ZY, Ba GJ. Determination of content of cinnamaldehyde in Shenggui
8 : 3107 oral liquid by HPLC [J]. China Pharm, 2007, 16(4): 35 37. [7],,. [J]., 2008, 28(9): 1559 1561. Li XN, Ge X, Li QS. High performance liquid chromatography determination of cinnamaldehyde in Zushima Fengshi plaster [J]. J Pharm Anal, 2008, 28(9): 1559 1561. [8],. [J]., 2006, 10(2): 39 40. Li YK, Zhang YQ. Determination of cinnamaldehyde in yinaofang oral liquid by HPLC [J]. Anhui Med Pharm J, 2006, 10(2): 39 40. [9],,. HPLC [J]., 2007, 24(6): 39 41. Liu Q, Deng Y, Nan JL. Determination of content of cinnamaldehyde in Guizhi spray by HPLC [J]. J Gansu Coll Tradit Chin Med, 2007, 24(6): 39 41. [10],. HPLC [J]., 2009, 26(4): 19 20. Wang LZ, Jiang WQ. Determination of cinnamaldehyde and cinnamic acid in cassia twig by HPLC [J]. Tradit Chin Med Inf, 2009, 26(4): 19 20. [11],,. [J]., 2000, 9(25): 544 545. Luo JP, Zhang ZS, Tian C. Determination of content of cinnamaldehyde in Shenggui oral liquid by HPLC [J]. Chin J Tradit Chin Med, 2000, 9(25): 544 545. [12],,,. [J]., 2013, 4(2): 463 466. Cao JM, Guo CY, Liu DP, et al. Determination of content of cinnamaldehyde in cassia twig by HPLC [J]. J Food Saf Qual, 2013, 4(2): 463 466. [13],,,. RP-HPLC [J]., 2008, 10(4): 9 11. Ma RR, Tang YH, Sun ZL, et al. Determination of cinnamaldehyde and cinnamic acid in cortex cinnamomi from different habits by RP-HPLC [J]. Chin Mod Tradit Chin Med, 2008, 10(4): 9 11. [14],,,. [J]., 2005, 40(23): 93 95. Lin J, Xu LZ, Liu JY, et al. Study on contents of cinnamaldehyde and cinnamic acid and distribution of cassia twig [J]. Chin J Pharm Sci, 2005, 40(23): 93 95. [15],. HPLC [J]., 2008, 26(2): 50 53. Zhong JJ, Yang XF. Determination of cinnamaldehyde in Guifudihuang pills by HPLC [J]. Chin Archives Tradit Chin Med, 2008, 26(2): 50 53. [16],,. [J]., 2012, (9): 45 50. Xie YX, Li M, Wang SH. Determination of cinnamaldehyde in Shengui capsules by HPLC [J]. Pharm Today, 2012, (9): 45 50. [17],,. HPLC [J]., 2008, 28(1): 124 125. Xu ZM, Han YT, Zhao XY. HPLC determination of cinnamaldehyde in Sanhan Huoxue plaster [J]. J Anal, 2008, 28(1): 124 125. [18],,. HPLC [J]., 2012, 24(4): 59 61. Liu Y, Xie M, Wu CM. HPLC fingerprint analysis of cinnamon from different origins and study on the contents of cinnamaldehyde [J]. Strait Pharm, 2012, 24(4): 59 61. [19],,. HPLC [J]., 2010, 45(21): 1664 1666. Chen HM, Wu CM, Xie M. Simultaneous determination of cumarin, cinnamyl alcohol,cinnamic acid and cinnamaldehyde in cortex cinnamomi by HPLC [J]. Chin J Pharm Sci, 2010, 45(21): 1664 1666. [20],. HPLC [J]., 2008, 31(7): 1086 1087. Xie M, Zhang QP. Determination of cinnamaldehyde in gastric powder by HPLC [J]. Tradit Chin Med Mater, 2008, 31(7): 1086 1087. [21],,,. HPLC [J]., 2010, 12(2): 39 41. Song LH, Zhang R, Wan HJ, et al. Determination of cinnamaldehyde in guizhifuling tablets by HPLC [J]. J Hubei Coll Tradit Chin Med, 2010, 12(2): 39 41. [22]. HPLC [J]., 2014, 5(8): 15 16. Liu JB. Determination of cinnamaldehyde in Yougui pill by HPLC [J]. Heilongjiang Sci, 2014, 5(8): 15 16. 作者简介 ( 责任编辑 : 刘丹 ) 梁国华, 副主任药师, 主要研究方向为食品安全检测 E-mail: lgh1280@sina.com