固体复合香辛料中罂粟壳质控样的制备
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摘要
建立了一种固体复合香辛料中罂粟壳质控样制备方法。将香辛料基质材料与罂粟壳各自经微波干燥、混合、粉碎和过筛,后经一次混合、加抗结剂、二次干燥、二次过筛和二次混合后,制得200份质控样本。经均匀性与稳定性检验后,由10家实验室采用液相色谱-串联质谱法对样本进行协同定值,并进行不确定度评估。结果表明:样本中5种生物碱类物质的特性值分别为可待因(907±20.9)μg/kg,蒂巴因(918±18.4)μg/kg,吗啡(315±16.5)μg/kg,罂粟碱(171±12.6)μg/kg,那可丁(139±15. 8)μg/kg,均匀性与稳定性良好,适用于复合香辛料中生物碱类物质检测过程的方法验证与质量控制。
To establish a method for quality control samples for the poppy shell in solid compound spices.The spice matrix materials and the poppy shell were dried by microwave,mixed,pulverized,sieved,and then mixed again. After added with antagonist,the samples were dried,sieved, and mixed again. The homogeneity and stability of the samples were strictly examined. The concentrations of each chemical constituent in the samples were collaboratively analyzed using liquid chromatography-tandem mass spectrometry in 10 laboratories and then the uncertainty was assessed. The results showed that the characteristic values of the codeine, thebaine, morphine, papaverine, noscapine in these samples were(907 ±20.9),(918 ± 18. 4),(315 ± 16. 5),( 171 ± 12. 6),( 139 ± 15. 8) μg/kg respectively. The uniformity and stability was good. The methodology is suitable for verifying alkaloids in solid compound spices to control the quality.
To establish a method for quality control samples for the poppy shell in solid compound spices.The spice matrix materials and the poppy shell were dried by microwave,mixed,pulverized,sieved,and then mixed again. After added with antagonist,the samples were dried,sieved, and mixed again. The homogeneity and stability of the samples were strictly examined. The concentrations of each chemical constituent in the samples were collaboratively analyzed using liquid chromatography-tandem mass spectrometry in 10 laboratories and then the uncertainty was assessed. The results showed that the characteristic values of the codeine, thebaine, morphine, papaverine, noscapine in these samples were(907 ±20.9),(918 ± 18. 4),(315 ± 16. 5),( 171 ± 12. 6),( 139 ± 15. 8) μg/kg respectively. The uniformity and stability was good. The methodology is suitable for verifying alkaloids in solid compound spices to control the quality.
引文
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[16]刘亚雄,刘丛丛,庄玥,等.基于电子鼻技术对调味品中非法添加罂粟壳的检测[J].中国食物与营养,2017,7(3):81-85.LIU Y C,LIU C C,ZHUANG Y, et al. Detection of condiments illegally added by pericarpium papaveris using electronic nose[J]. Food and Nutrition in China,2017,7(3):81-85.
[17]朱德泉,王继先,朱德文,等.小麦微波干燥特性及其对品质的影响[J].农业工程学报,2006,22(4):182-185.ZHU D Q,WANG J X,ZHU D W,et al. Experimental study on wheat grain microwave drying characteristics and its effect on the quality of wheat grain[J]. Transactions of the CSAE,2006,22(4):182-185.
[18]赵超,陈建,邱兵,等.花椒微波干燥特性试验[J].农业机械学报,2007,38(3):98-101.ZHAO C,CHEN J, QIU B, et al. Experimental study on microwave drying characteristics of Chinese prickly ash[J]. Transactions of the CSAM, 2007,38(3):98-101.
[2]杨铭铎,于洋.复合调味料的研究进展[J].黑龙江科学,2017,8(21):156-159.YANG M D,YU Y. The research progress of compound seasoning[J]. Heilongjiang Science, 2017,8(21):156-159.
[3]陈洪榕,陈巧玲.中国食品安全档案[M].北京:金盾出版社,2015:259-262.CHEN H R,CHEN Q L. China food safety archives[M].Beijing:Golden Shield Press,2015:259-262.
[4]谢志浩.健康产品中非法添加化学成分快速筛查方法理论与实践[M].广州:华南理工大学出版社,2011:1166-1169.XIE Z H. Theory and practice of rapid screening method for illegally added chemical constituents in health products[M]. Guangzhou:South China University of Technology Press,2011:1166-1169.
[5] SAMIRAN P, ANINDYA C, CHANDAN S, et al. Morphine and codeine in the water extract of poppy straw:a traditional substitution used by drug users in Calcutta, India[J]. International Journal of Drug Policy,2003, 10(4):214-216.
[6]李雕,李进瞳,曾燕,等.不同等级罂粟壳有效成分含量的研究[J].中国中药杂志,2010,35(17):2246-2249.LI D,LI J T,ZENG Y,et al. Study on the contents of active components in different grade of poppy[J]. China Journal of Chinese Materia Medica, 2010, 35(17):2246-2249.
[7]中华人民共和国国家卫生和计划生育委员会.食品中可能违法添加的非食用物质和易滥用的食品添加剂名单(第1-5批汇总)[EB/OL].(2011-04-19)[2017-04-22]. http://www. nhfpc. gov. cn/zwgkzt/wsbysj/201104/51441. shtml.
[8]皮立,胡凤祖,师治贤.高效液相色谱-荧光检测法测定罂粟籽和火锅汤料中的罂粟碱[J].色谱,2005,23(6):639.PI L,HU F Z,SHI Z X. Determination of papaverine in seeds of Papaver Somniferum L. and soup of chafing dish by high performance liquid chromatography-fluorescence detection[J]. Chinese Journal of Chromatography,2005,23(6):639.
[9]林黛琴,王婷婷,万承波,等.高效液相色谱-串联质谱法快速测定食品中5种罂粟壳生物碱[J].质谱学报,2017,2(38):239-247.LIN D Q,WANG T T,WAN C B,et al. Rapid determination of five opium poppy husk alkaloids in foods by HPLC-MS/MS[J]. Journal of Chinese Mass Spectrometry Society,2017,2(38):239-247.
[10]乔庆东.火锅底料中5种生物碱含量的高效液相色谱-三重四级杆串联质谱测定法[J].职业与健康,2017,9(33):2483-2493.QIAO Q D. Determination of 5 alkaloids in hot pot condiment by high performance liquid chromatography-electrospray tandem mass spectrometry[J]. Occupation and Health,2017,9(33):2483-2493.
[11]张百乐,高黎红,解迎双,等.实时直接分析-串联质谱法快速筛查火锅底料、牛肉面汤及调味料中罂粟壳生物碱[J].职业与健康,2017,7(35):724-729.ZHANG B L,GAO L H,XIE Y S, et al. Rapid screening the alkaloids of poppy shell in hot pot condiment,beef noodle soup and seasoning by direct analysis in real time-tandem mass spectrometry[J]. Occupation and Health,2017,7(35):724-729.
[12] REDDY M M, SUMSH V, JAYASHANKER G, et al.Application of capillary zone electrophoresis in the sepa-ration and determination of the principal gum opiumalkaloids[J]. Electrophoresis, 2003,24(9):1437-1441.
[13]沈平,谢朝梅,谢燕湘,等.GC-MS法直接测定食品中罂粟壳提取物的残留量[J].中国卫生检验杂志,2015,25(20):3466-3468.SHEN P,XIE C M,XIE Y X, et al. Direct determination of residues of poppy shell extracts in food by GC MS[J]. China Journal of Health Laboratory Technology,2015,25(20):3466-3468.
[14]刘洋,张辉,陆志芸,等.复合调味粉中罂粟成分的实时荧光PCR检测方法[J].中国调味品,2011,7(36):93-96.LIU Y,ZHANG H,LU Z Y,et al. A method of real-time PCR for detection of Papaver somniferumin in mixed seasoning powder[J]. China Condiment, 2011,7(36):93-96.
[15]朱振华,朱士新,陈璐,等.罂粟壳成分快速检测方法在食品监督中的应用[J].中国食物与营养,2015,21(3):8-10.ZHU Z H,ZHU S X,CHEN L,et al. Application of rapid detection method of poppy shell components in food supervision[J]. Food and Nutrition in China, 2015,21(3):8-10.
[16]刘亚雄,刘丛丛,庄玥,等.基于电子鼻技术对调味品中非法添加罂粟壳的检测[J].中国食物与营养,2017,7(3):81-85.LIU Y C,LIU C C,ZHUANG Y, et al. Detection of condiments illegally added by pericarpium papaveris using electronic nose[J]. Food and Nutrition in China,2017,7(3):81-85.
[17]朱德泉,王继先,朱德文,等.小麦微波干燥特性及其对品质的影响[J].农业工程学报,2006,22(4):182-185.ZHU D Q,WANG J X,ZHU D W,et al. Experimental study on wheat grain microwave drying characteristics and its effect on the quality of wheat grain[J]. Transactions of the CSAE,2006,22(4):182-185.
[18]赵超,陈建,邱兵,等.花椒微波干燥特性试验[J].农业机械学报,2007,38(3):98-101.ZHAO C,CHEN J, QIU B, et al. Experimental study on microwave drying characteristics of Chinese prickly ash[J]. Transactions of the CSAM, 2007,38(3):98-101.