Microsoft Word 张喜金-二校出3109、3111

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1 6 8 Vol. 6 No Journal of Food Safety and Quality Aug., 2015 张喜金 *, 苏昭仑, 黄康惠 (, ) 摘要 : 目的方法, / (V:V=60:40), 1.2 ml/min, Waters Spherisorb C 18, 40 ; 203 nm 结果 ~ mg/ml, r>0.999, %,, 100.5%, 0.6%(n=9) WS-1001-(HD )-2002, 结论,, 关键词 : ; ; Determination of squalene in squalene soft capsule by high performance liquid chromatography ZHANG Xi-Jin *, SU Zhao-Lun, HUANG Kang-Hui (By-Health Co., Ltd., Zhuhai , China) ABSTRACT: Objective To establish a method for the determination of squalene in squalene soft capsules by high performance liquid chromatography. Methods Samples were extracted with methanol, and being separated by waters spherisorb C 18 column with the mobile phase of methanol/acetonitrile (V:V=60:40), and the flow rate was 1.2 ml/min, the column temperature was 40, the content of squalene were determined by HPLC under the detection wavelength at 203 nm. Results The method showed a good linearity in the range of ~ mg/ml for squalene with the coefficient r>0.999, the detection limit was %, the average recovery of different adding levels was 100.5%, and the relative standard deviation was 0.6%(n=9). Compared with the WS-1001-(HD )-2002 squalene gas chromatography method of National Drug Standards, there was no statistical difference between the two results. Conclusion HPLC method is more quick and easy, saving testing cost, and applicable to measure the content of squalene in health foods. KEY WORDS: squalene; high performance liquid chromatography; health food 1 引言,, 1914 squalene, 2,6,10,15,19,23- -2,6,10,14,18,22-,,, (SOD), [1-5] * 通讯作者 :, @qq.com *Corresponding author: ZHANG Xi-Jin, By-Health Co., Ltd., Zhuhai , China @qq.com

2 8, : 3109,,,,,, [6-8],,,,,,, 2 材料与方法 2.1 实验仪器 15C ( ), C 18 (5 μm, 4.6 mm 150 mm), XP-205 ( ) 2.2 标准与试剂 (SUPELCO, 99.0%), (, 2) 2.3 色谱条件液相色谱条件 : Waters Sphrisorb C 18 (5 μm, 4.6 mm 150 mm); : 40 ; : 203 nm; : 1.2 ml/min; : - (V:V=60:40) 气相色谱条件 : Agilent 7890A, FID( ); : 280, 10:1, 1 μl; : Agilent, HP-5, 30 m 320 μm 0.25 μm, 2 ml/min; : 250, 14 min; : 280, 30 ml/min, 400 ml/min, 30 ml/min 2.4 对照品溶液的制备 mg 10 ml,, ml 10 ml, mg/ml 2.5 样品溶液的制备 mg( 0.01 mg) 50 ml,,,, 0.45 μm, 3 结果与讨论 3.1 色谱条件选择波长的选择 ( 1) 203 nm,, 203 nm, 203 nm 流动相和柱温选择,,,, /, : =60:40(V:V), nm, ml/min 30 40, : =60:40(V:V) 203 nm 1.2 ml/min 40, min, 3.2 方法性能指标工作曲线和线性范围, 5,, 0.10 mg/ml 0.50 mg/ml [9,10] Y= X-0.021, r 2 =0.9999, GB/T , GB/T r [11] 检出限实验, (S/N) 3, μg/ml, 10 mg,

3 Fig. 1 1 Ultraviolet absorption curve of squalene standard Fig. 2 2 Chromatogram of squalene standard Fig. 3 3 Chromatogram of the sample

4 8, : 3111 Tapble 1 表 1 对照品浓度与峰面积的关系 The relationship between the concentration of the reference and the peak area /mg ml -1 STD STD STD STD STD Y= X (r 2 ) Fig. 4 4 Standard curve of squalene 50 ml, % 重复性实验 ( E), 6, 10 mg, 2.5, 2.3, 98.5%, RSD 0.2% 供试品含量测定 3, 2.5, 2.3, 回收率实验 mg ( 98.5 %)( 9 ), 50mL, ( mg/ml)2.4 ml 3.0 ml 3.6 ml,,, 0.45 μm, %, (RSD) 0.6 %, GB/T ( ) [11-14], 稳定性实验, h,, RSD 0.2 % (n=6), 48 h Taple 2 表 2 不同样品中角鲨烯含量测定结果 Squalene content determination results in different samples /mg -1 / % E Table 3 表 3 回收率实验 The recovery of experiment /mg /mg /mg /% /% RSD/%

5 方法验证, WS-1001-(HD )-2002 :,, [15] 4, 2, 2 WS-1001-(HD )- 2002,, t, (t=0.202, P >0.10), 4 表 4 液相色谱法与气相色谱法的对比 (%) Taple 4 Comparison of the liquid chromatography and gas chromatography (%) 5 结论 % 98.45% % 98.01% % 99.33% % 98.37% % 99.32% % 98.39% % 97.55% % 98.69%, Waters SpherisorbC 18, / (60/40=V:V),,,, WS-1001-(HD )-2002,, 2, 2,,, 参考文献 [1] [EB/OL]. ( ). National Scientific and Technical Terms of Validation Committee[EB/OL]. ( ). [2],,,. [J]., 1990, 2: Zhou JX, Li XY, Tang BD, et al. Anti-tumor and immunomodulatory effects of squalene [J]. Chin J Pharm Toxi, 1990, 2: [3]. [J]., 2002, 23(1): Pan F. Squalene secret to improving the quality of human life [J]. Shanghai Med, 2002, 23(1): [4],. [J]., 2004, 24(3): Zhao ZD, Sun Z. Research progress and application of resources hound fish bioactive substances [J]. Chem Ind Forest Prod, 2004, 24(3): [5],,,. [J]., 2005, 35: Xu RB, Liu WW, Wang MY, et al. The progress of preparation and application of squalene [J]. Chin J Shandong Med, 2005, 45(35): [6],. [J]., 2008, 29(2): CheXiY, LuW. Determination of squalene in squalene soft capsules by gas chromatography [J]. J Qiqihar Med Coll, 2008, 29(12): [7],. [J]., 2002, 9 (6): Li Q,ZhouSP.Determination of squalene by gas chromatography [J]. Capital Med, 2002, 9(6): [8],,. \ [J]., 2000, 23(1): 11. Mou ZC, Zhang JW, Zhang CJ. Determination of squalene health products by gas chromatography, purity [J]. Chin J Health Quarantine, 2000, 23(1): 11. [9],,. [J]., 2010, 8: Liang XH, Zheng CX, Zhang FX. Extraction and HPLC Analysis of the Squalene in Gly-cyrrhiza uralensis Fisch [J]. Chin J Lishizhen Med Mater Med Res, 2010, 21:

6 8, : 3113 [10],,,. [J]., 2006, 2: Chen QB, Cheng ZQ, Yang JX, et al. The HPLC analysis of the squalene in Siraitia grosvenorii seed oil [J]. Chin J Guangxi Sci, 2006, 13: [11] GB/T [S] GB/T Criterion on quality control of laboratories-chemical testing of food [S]. [12]. [D]. :, Dai YH. Research on separation and extraction of squalene from olive oil [D]. Tianjin: Tianjin University, [13]. [D]. :, Qi DZ. Research on separation and extraction of squalene from SODD [D]. Tianjin: Tianjin University, [14]. [D]. :, Cheng ZQ. The Study on separation,purification of luohanguo squalene and lipidic components of Luohanguo residue [D]. Guilin: Guangxi Normal University, [15] WS-1001-(HD )-2002 [C]. WS-1001-(HD )-2002 by National Drug Standards [C]. 作者简介 ( 责任编辑 : 白洪健 ) 张喜金, 主要研究方向为保健食品的质量检测 @qq.com

Microsoft Word - 3098-3102 20150611007-蔡伟江-二校

Microsoft Word - 3098-3102 20150611007-蔡伟江-二校 6 8 Vol. 6 No. 8 2015 8 Journal of Food Safety and Quality Aug., 2015 蔡伟江 *, 邓鹏飞, 刘光兰, 李丹 (, 519040) 摘要 : 目的, 方法 (4.6 mm 250 mm, 5.0 μm) ; : : : =70: 16: 14(V:V:V),, : 1.0 ml/min; : 40 ; : 10

Microsoft Word 张喜金-二校 出3109、3111

Microsoft Word 张喜金-二校出3109、3111