干旱区生态环境知识资源中心(Arid): 固相萃取柱净化-超高效液相色谱-串联质谱法测定助眠类保健品中22种禁用安神类药物的含量

Arid

	固相萃取柱净化-超高效液相色谱-串联质谱法测定助眠类保健品中22种禁用安神类药物的含量
其他题名	UPLC-MS/MS Determination of 22Forbidden Sedative-Hypnotics in Sleep-Aiding Health Care Products with SPE Column Purification
	钟世欢; 金建奇; 叶磊海; 叶佳明; 王潇; 裘钧陶
来源期刊	理化检验. B, 化学分册
ISSN	1001-4020
出版年	2020
卷号	56 期号:1
中文摘要	应用超高效液相色谱-串联质谱法测定了助眠类保健品中22种禁用安神类药物的含量。将样品连同其包衣和胶囊壳一起研碎后称取1.000g样品用甲醇溶解, 经涡旋混匀并超声15min,用甲醇定容至25.0mL。离心后取上清液5.00mL,经Oasis PRiME HLB固相萃取柱净化处理,收集经净化的流出液,与用于淋洗固相萃取柱的甲醇2mL合并,于40℃下吹氮至溶液近干。用体积比为1∶1的0.05%(体积分数,下同)甲酸-甲醇混合溶液1.00mL溶解残渣,所得溶液经过0.22mum滤膜过滤,滤液供色谱分离。选用Poroshell120EC-C_( 18)色谱柱(50mm*3.0mm,2.7mum)作为固定相,用不同比例的(A)含0.05%甲酸的5mmol·L~(-1)乙酸铵溶液和(B)乙腈的混合溶液作为流动相按程序进行梯度洗脱。质谱测定中采用电喷雾离子源和多反应监测模式。结果表明:22种禁用安神类药物的标准曲线中有17种线性范围为 4~800mug·L~(-1),有1种为40~8000mug·L~(-1),还有4种为400~80000mug·L~(-1),其检出限(3S/N )为0.02~2mug·g~(-1)。用标准加入法进行回收试验,测得回收率为81.2%~98.9%,测定值的相对标准偏差(n=6)为3.1%~9 .7%。
英文摘要	UPLC-MS/MS was applied to the determination of 22 forbidden sedative-hypnotics in some sleepaiding health care products.Sample for analysis was prepared by grinding the health care food itself together with its capsula into powder and a portion of 1.000g was taken and dissolved in methanol with aid of ultrasonic treatment for 15min.The solution was diluted to 25.0 mL with methanol and centrifuged.An aliquot of 5.00 mL of the supernatant was taken and purified by passing through the Oasis PRiME HLB SPE column.The eluate from the SPE column was collected and mixed with the methanol(2mL)used in washing the column.The mixed solution was then evaporated to neardryness by N_2-blowing at 40℃.The residue was taken up with 1.00mL of a mixed solution of 0.005%(volume fraction,same as below)formic acid-methanol with the volume ratio of 1∶1,and the solution was filtered through 0.22mum filtering membrane and the filtrate was used for UPLC separation by passing through Poroshell 120EC-C_(18) chromatographic column(50mm*3.0 mm,2.7mum)as stationary phase,and mixture of(A)5mmol·L~(-1) NH_4OAc solution(containting 0.05%formic acid)and(B)acetonitrile in various ratios were used as mobile phases in gradient elution.In MS/MS determination,ESI and MRM mode were adopted.It was shown that among the standard curves of the 22 forbidden sedative-hypnotics,linearity ranges for 17sedativehypnotics were same between 4mug·L~(-1) and 800mug·L~(-1),for one sedative-hypnotic between 40mug·L~(-1) and 8 000mug·L~(-1) and for the remaider 4sedative-hypnotics between 400mug·L~(-1) and 80 000mug·L~(-1);the detection limits(3S/N)found for these sedative-hypnotics were in the range of 0.02-2mug·g~(-1).Recovery was tested by standard addition method,giving values of recovery in the range of 81.2%-98.9%,and values of RSDs(n=6)in the range of 3.1%-9.7%.
中文关键词	超高效液相色谱-串联质谱法 ; 固相萃取柱净化 ; 禁用安神类药物 ; 助眠类保健品
英文关键词	UPLC-MS/MS SPE column purification forbidden sedative-hypnotic sleep-aiding health care product
类型	Article
语种	中文
收录类别	CSCD
WOS类目	Chemistry
CSCD记录号	CSCD:6670958
资源类型	期刊论文
条目标识符	http://119.78.100.177/qdio/handle/2XILL650/353648
作者单位	钟世欢, 赞宇科技集团股份有限公司, 杭州, 浙江 310009, 中国. 金建奇, 浙江金正检测有限公司, 义乌, 321000. 叶磊海, 赞宇科技集团股份有限公司;;浙江公正检验中心有限公司, ;;, 杭州;;杭州, ;; 310009;;310009. 叶佳明, 浙江公正检验中心有限公司, 杭州, 浙江 310009, 中国. 王潇, 浙江公正检验中心有限公司, 杭州, 浙江 310009, 中国. 裘钧陶, 浙江公正检验中心有限公司, 杭州, 浙江 310009, 中国.
推荐引用方式 GB/T 7714	钟世欢,金建奇,叶磊海,等. 固相萃取柱净化-超高效液相色谱-串联质谱法测定助眠类保健品中22种禁用安神类药物的含量[J],2020,56(1).
APA	钟世欢,金建奇,叶磊海,叶佳明,王潇,&裘钧陶.(2020).固相萃取柱净化-超高效液相色谱-串联质谱法测定助眠类保健品中22种禁用安神类药物的含量.理化检验. B, 化学分册,56(1).
MLA	钟世欢,et al."固相萃取柱净化-超高效液相色谱-串联质谱法测定助眠类保健品中22种禁用安神类药物的含量".理化检验. B, 化学分册 56.1(2020).