中国药学杂志

t/min	B/%
0	20
0.5	20
1.5	40
3	60
13	98
14.5	98
14.6	20
17	20

t/min	B/%
0	20
0.5	20
1.5	40
3	60
13	98
14.5	98
14.6	20
17	20

No.	t_R /min	m/z (Average)	Glyceride	Formula	Adduct type	Mixture of GTS, GTP,GDP, GDS,GMP and GMS	Manufacture
1	2.946	348.311 08	MG 16∶0	C₁₉H₃₈O₄	[M+NH4]⁺	0.12%	0.48%	0.48%	0.55%	0.47%	0.73%	0.37%
2	3.443	376.342 02	MG 18∶0	C₂₁H₄₂O₄	[M+NH4]⁺	0.15%	0.83%	1.02%	0.79%	0.68%	1.16%	0.48%
3	3.880	404.373 05	MG 20∶0	C₂₃H₄₆O₄	[M+NH4]⁺	0.00%	0.03%	0.02%	0.02%	0.02%	0.02%	0.01%
4	5.030	530.477 57	DG 28∶0\|DG 12∶0_16∶0	C₃₁H₆₀O₅	[M+NH4]⁺	0.02%	0.34%	0.04%	0.08%	0.12%	0.03%	0.07%
5	5.477	558.508 58	DG 30∶0\|DG 14∶0_16∶0	C₃₃H₆₄O₅	[M+NH4]⁺	0.24%	0.98%	0.35%	0.57%	0.58%	0.23%	0.55%
6	5.972	586.539 87	DG 32∶0\|DG 16∶0_16∶0	C₃₅H₆₈O₅	[M+NH4]⁺	9.41%	11.98%	10.94%	12.12%	10.33%	15.15%	11.26%
7	6.488	614.571 39	DG 34∶0\|DG 16∶0_18∶0	C₃₇H₇₂O₅	[M+NH4]⁺	14.24%	19.61%	27.20%	19.28%	16.52%	30.48%	17.93%
8	6.752	628.586 85	DG 35∶0\|DG 17∶0_18∶0	C₃₈H₇₄O₅	[M+NH4]⁺	0.05%	0.08%	0.11%	0.06%	0.06%	0.12%	0.06%
9	7.014	642.602 54	DG 36∶0\|DG 18∶0_18∶0	C₃₉H₇₆O₅	[M+NH4]⁺	5.98%	8.73%	18.96%	8.70%	7.46%	15.91%	7.78%
10	7.544	670.633 47	DG 38∶0\|DG 18∶0_20∶0	C₄₁H₈₀O₅	[M+NH4]⁺	0.18%	0.29%	0.65%	0.30%	0.26%	0.42%	0.27%
11	8.062	698.666 18	DG 40∶0\|DG 16∶0_24∶0	C₄₃H₈₄O₅	[M+NH4]⁺	0.06%	0.48%	0.23%	0.14%	0.12%	0.11%	0.12%
12	8.062	698.664 98	DG 40∶0\|DG 18∶0_22∶0	C₄₃H₈₄O₅	[M+NH4]⁺	0.06%	0.83%	0.23%	0.14%	0.12%	0.11%	0.12%
13	9.389	796.738 16	TG 46∶0\|TG 14∶0_16∶0_16∶0	C₄₉H₉₄O₆	[M+NH4]⁺	1.08%	0.03%	1.00%	1.73%	2.19%	-	1.88%
14	9.822	824.769 38	TG 48∶0\|TG 16∶0_16∶0_16∶0	C₅₁H₉₈O₆	[M+NH4]⁺	18.17%	0.34%	5.67%	14.03%	15.64%	7.17%	15.87%
15	10.029	838.785 08	TG 49∶0\|TG 16∶0_16∶0_17∶0	C₅₂H₁₀₀O₆	[M+NH4]⁺	0.22%	0.98%	0.13%	0.18%	0.20%	0.15%	0.16%
16	10.232	852.800 42	TG 50∶0\|TG16∶0_16∶0_18∶0/TG 16∶0_18∶0_16∶0	C₅₃H₁₀₂O₆	[M+NH4]⁺	28.79%	11.98%	14.45%	23.37%	25.60%	14.61%	24.70%
17	10.421	866.815 67	TG 51∶0\|TG 16∶0_17∶0_18∶0	C₅₄H₁₀₄O₆	[M+NH4]⁺	0.17%	19.61%	0.09%	0.15%	0.13%	0.09%	0.13%
18	10.614	880.831 68	TG 52∶0\|TG 16∶0_18∶0_18∶0/TG 18∶0_16∶0_18∶0	C₅₅H₁₀₆O₆	[M+NH4]⁺	17.30%	0.08%	13.77%	14.50%	15.95%	10.74%	14.88%
19	10.971	908.863 1	TG 54∶0\|TG 18∶0_18∶0_18∶0	C₅₇H₁₁₀O₆	[M+NH4]⁺	3.74%	8.73%	4.65%	3.29%	3.55%	2.74%	3.36%

No.	t_R /min	m/z (Average)	Glyceride	Formula	Adduct type	Mixture of GTS, GTP,GDP, GDS,GMP and GMS	Manufacture
1	2.946	348.311 08	MG 16∶0	C₁₉H₃₈O₄	[M+NH4]⁺	0.12%	0.48%	0.48%	0.55%	0.47%	0.73%	0.37%
2	3.443	376.342 02	MG 18∶0	C₂₁H₄₂O₄	[M+NH4]⁺	0.15%	0.83%	1.02%	0.79%	0.68%	1.16%	0.48%
3	3.880	404.373 05	MG 20∶0	C₂₃H₄₆O₄	[M+NH4]⁺	0.00%	0.03%	0.02%	0.02%	0.02%	0.02%	0.01%
4	5.030	530.477 57	DG 28∶0\|DG 12∶0_16∶0	C₃₁H₆₀O₅	[M+NH4]⁺	0.02%	0.34%	0.04%	0.08%	0.12%	0.03%	0.07%
5	5.477	558.508 58	DG 30∶0\|DG 14∶0_16∶0	C₃₃H₆₄O₅	[M+NH4]⁺	0.24%	0.98%	0.35%	0.57%	0.58%	0.23%	0.55%
6	5.972	586.539 87	DG 32∶0\|DG 16∶0_16∶0	C₃₅H₆₈O₅	[M+NH4]⁺	9.41%	11.98%	10.94%	12.12%	10.33%	15.15%	11.26%
7	6.488	614.571 39	DG 34∶0\|DG 16∶0_18∶0	C₃₇H₇₂O₅	[M+NH4]⁺	14.24%	19.61%	27.20%	19.28%	16.52%	30.48%	17.93%
8	6.752	628.586 85	DG 35∶0\|DG 17∶0_18∶0	C₃₈H₇₄O₅	[M+NH4]⁺	0.05%	0.08%	0.11%	0.06%	0.06%	0.12%	0.06%
9	7.014	642.602 54	DG 36∶0\|DG 18∶0_18∶0	C₃₉H₇₆O₅	[M+NH4]⁺	5.98%	8.73%	18.96%	8.70%	7.46%	15.91%	7.78%
10	7.544	670.633 47	DG 38∶0\|DG 18∶0_20∶0	C₄₁H₈₀O₅	[M+NH4]⁺	0.18%	0.29%	0.65%	0.30%	0.26%	0.42%	0.27%
11	8.062	698.666 18	DG 40∶0\|DG 16∶0_24∶0	C₄₃H₈₄O₅	[M+NH4]⁺	0.06%	0.48%	0.23%	0.14%	0.12%	0.11%	0.12%
12	8.062	698.664 98	DG 40∶0\|DG 18∶0_22∶0	C₄₃H₈₄O₅	[M+NH4]⁺	0.06%	0.83%	0.23%	0.14%	0.12%	0.11%	0.12%
13	9.389	796.738 16	TG 46∶0\|TG 14∶0_16∶0_16∶0	C₄₉H₉₄O₆	[M+NH4]⁺	1.08%	0.03%	1.00%	1.73%	2.19%	-	1.88%
14	9.822	824.769 38	TG 48∶0\|TG 16∶0_16∶0_16∶0	C₅₁H₉₈O₆	[M+NH4]⁺	18.17%	0.34%	5.67%	14.03%	15.64%	7.17%	15.87%
15	10.029	838.785 08	TG 49∶0\|TG 16∶0_16∶0_17∶0	C₅₂H₁₀₀O₆	[M+NH4]⁺	0.22%	0.98%	0.13%	0.18%	0.20%	0.15%	0.16%
16	10.232	852.800 42	TG 50∶0\|TG16∶0_16∶0_18∶0/TG 16∶0_18∶0_16∶0	C₅₃H₁₀₂O₆	[M+NH4]⁺	28.79%	11.98%	14.45%	23.37%	25.60%	14.61%	24.70%
17	10.421	866.815 67	TG 51∶0\|TG 16∶0_17∶0_18∶0	C₅₄H₁₀₄O₆	[M+NH4]⁺	0.17%	19.61%	0.09%	0.15%	0.13%	0.09%	0.13%
18	10.614	880.831 68	TG 52∶0\|TG 16∶0_18∶0_18∶0/TG 18∶0_16∶0_18∶0	C₅₅H₁₀₆O₆	[M+NH4]⁺	17.30%	0.08%	13.77%	14.50%	15.95%	10.74%	14.88%
19	10.971	908.863 1	TG 54∶0\|TG 18∶0_18∶0_18∶0	C₅₇H₁₁₀O₆	[M+NH4]⁺	3.74%	8.73%	4.65%	3.29%	3.55%	2.74%	3.36%

LC-TOF-MS法测定6种不同来源的单双硬脂酸甘油酯组成

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陈雷霖 ¹ , 付蒙 ¹ , 周茜 ¹ , 鲍实 ¹ , 曹运姣 ² , 王宇帆 ³ , 查海红 ⁴ , 刘晨曦 ¹^,^* , 胡敏 ¹^,^*

中国药学杂志 | 论著 2025,60(9): 995-999

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中国药学杂志 | 论著 2025, 60(9): 995-999

LC-TOF-MS法测定6种不同来源的单双硬脂酸甘油酯组成

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陈雷霖¹, 付蒙¹, 周茜¹, 鲍实¹, 曹运姣², 王宇帆³, 查海红⁴, 刘晨曦¹^,^*, 胡敏¹^,^*

作者信息

¹ 湖北省药品监督检验研究院, 湖北省药品质量检测与控制工程技术研究中心, 武汉 430075

² 湖北中医药大学, 武汉 430065

³ 湖北省药品监督管理局药品审评检查中心, 武汉 430077

⁴ 上海爱博才思分析仪器贸易有限公司, 上海 200335

陈雷霖,男,硕士,药师研究方向:药品质量控制;

付蒙,女,硕士,主管药师研究方向:药品质量控制。陈雷霖和付蒙为共同第一作者

通讯作者:

^*胡敏,女,硕士,正高级工程师研究方向:药品刘晨曦,男,硕士,主管药师研究方向:药品质量控制 Tel:(027)87705266

刘晨曦,男,硕士,主管药师研究方向:药品质量控制 Tel:(027)87705266

Identification and Characterization of the Composition of Glyceryl Mono- and Distearate from Six Different Sources by LC-TOF-MS

Leilin CHEN¹, Meng FU¹, Qian ZHOU¹, Shi BAO¹, Yunjiao CAO², Yufan WANG³, Haihong ZHA⁴, Chenxi LIU¹^,^*, Min HU¹^,^*

Affiliations

¹ Hubei Engineering Research Center for Drug Ouality Control, Hubei Institute for Drug Control, Wuhan 430075, China

² Hubei University of Chinese Medicine, Wuhan 430065, China

³ HuBei Drug Administration Center for Drug Evaluation and Inspection, Wuhan 430077, China

⁴ SCIEX, Analytical Instrument Trading Co., Ltd., Shanghai 200335, China

出版时间: 2025-05-01 doi: 10.11669/cpj.2025.09.012

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摘要

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目的建立液相色谱-飞行时间质谱联用(LC-TOF-MS)法分析6种不同来源单双硬脂酸甘油酯样品中的甘油酯组成。方法采用四氢呋喃直接溶解样品,以Kinetex C₁₈色谱柱(2.1 mm×100 mm,2.6 μm)为分析柱,以甲醇-乙腈-水(1∶1∶1,含5 mmol·L^-1乙酸铵)为流动相A,异丙醇(含5 mmol·L^-1乙酸铵)为流动相B,流速为0.3 mL·min^-1,梯度洗脱。在电喷雾正负离子全扫描(TIC)模式下进行分析,采用面积归一化法定量,测定6种不同来源样品的单双硬脂酸甘油酯的19种脂肪酸甘油酯的组成和比例。结果不同来源的样品中甘油酯组成比例存在差异。结论本法可用于不同来源单双硬脂酸甘油酯的组分分析,为其质量等同性的内在机制研究提供了参考。

关键词

单双硬脂酸甘油酯 / 棕榈酸甘油酯 / 硬脂酸甘油酯 / 液相色谱-飞行时间质谱联用法

Abstract

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OBJECTIVE To identify the composition of glyceryl mono-and distearate (GMD) from different sources using an LC-TOF-MS method and compare the composition and proportion of glycerides in samples. METHODS A Kinetex C₁₈ column (2.1 mm×100 mm, 2.6 μm) was used as analysis column. Methanol-acetonitrile-water(1∶1∶1, containing 5 mmol·L^-1 ammonium acetate) was used as mobile phase A, and isopropanol(containing 5 mmol·L^-1 ammonium acetate) was used as mobile phase B, gradient elution was performed at a flow rate of 0.3 mL·min^-1. The analysis was carried out in ESI positive and negative ion full scanning(TIC) mode and quantified by area normalization method. RESULTS The composition and proportion of 19 fatty acid glycerides in six different sources of GMD showed significant differences in the composition and proportion of glycerides. CONCLUSION This method can be used to determine the composition and proportion of glycerides from different sources, thus contributing to the revelation of the internal mechanism affecting the quality equivalence of GMD.

Key words

glyceryl mono- and distearate / glyceryl palmitate / glyceryl stearate / LC-TOF-MS

引用本文

陈雷霖, 付蒙, 周茜, 鲍实, 曹运姣, 王宇帆, 查海红, 刘晨曦, 胡敏. LC-TOF-MS法测定6种不同来源的单双硬脂酸甘油酯组成. 中国药学杂志, 2025 , 60 (9) : 995 -999 . DOI: 10.11669/cpj.2025.09.012

Leilin CHEN, Meng FU, Qian ZHOU, Shi BAO, Yunjiao CAO, Yufan WANG, Haihong ZHA, Chenxi LIU, Min HU. Identification and Characterization of the Composition of Glyceryl Mono- and Distearate from Six Different Sources by LC-TOF-MS[J]. Chinese Pharmaceutical Journal, 2025 , 60 (9) : 995 -999 . DOI: 10.11669/cpj.2025.09.012

正文

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单双硬脂酸甘油酯(以下简称“单双甘油酯”),由于具有良好的乳化分散和增稠稳定作用,在乳剂、眼药膏等油/水型或水/油型乳化系的药品领域有广泛应用,它能够提高分散相的分散度,使其具有润肤、调理、防光、乳化以及滑爽的作用,同时保证产品的质量稳定。1853年,Berthelot首次在实验室采用甘油与硬脂酸直接酯化制得甘油单、双硬脂酸酯;1929年美国实现工业化生产,采用食用动植物油脂与甘油经催化醇解制备甘油单、双硬脂酸酯^[1]。《中国药典》2020年版四部将单双甘油酯定义为“单、二、三硬脂酸和棕榈酸混合甘油酯”^[2]。主要控制单甘油酯、二甘油酯、三甘油酯和游离甘油的含量。由于合成单双甘油酯的硬脂酸包含硬脂酸 50、硬脂酸 70和硬脂酸90 3种型号^[3],每种型号的硬脂酸中,硬脂酸和棕榈酸的含量均不相同。本品为硬脂酸和棕榈酸与甘油成酯以后形成的混合物,仅控制单甘油酯、二甘油酯和三甘油酯的总含量并不能准确反映产品的真实质量。

笔者对部分省内生产企业调研发现,不同来源的单双甘油酯对半固体制剂的成型效果有较大影响,甚至还会导致乳膏剂破乳,严重影响产品质量。

现行《中国药典》2020年版方法只能分离三甘油酯和二甘油酯,无法分离单甘油酯与游离脂肪酸,不能分析不同脂肪酸与甘油成酯的情况,存在测定方法专属性不强、准确度不高的问题。类似产品《日本药局方》第18版仅收载单硬脂酸甘油酯^[4],未对具体含量进行控制,仅列出性状、鉴别、理化检查等基础性项目。《美国药典》(USP)2024版^[5-7]是分成单、双、三甘油酯3个品种分别单独收载的,均采用示差折光检测器(differential refractive index detector,RID),以四氢呋喃为流动相,使用刚性苯乙烯-二乙烯苯共聚物微球填料柱对三、二、单甘油酯的含量进行测定。各国药典对其脂肪酸和脂质组分的分离测定并没有一个好的办法,其含量测定目前还存在分离度不佳、测定成分不明确的缺陷。关于单双甘油酯的组分分析方法国内外都鲜有文献报道^[8]。

本研究以药用半固体制剂的核心辅料单双甘油酯为对象,聚焦其甘油酯组成,通过建立液相色谱-飞行时间质谱联用(LC-TOF-MS)法测定其脂肪酸甘油酯的组成^[9-17],为其质量等同性的内在机制研究提供参考。

1 仪器与试药

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1.1 仪器

Zeno-TOF 7600型液相色谱质谱联用仪(SCIEX公司);XS205型分析天平(梅特勒·托利多仪器有限责任公司)。

1.2 试药

水为自制超纯水;乙酸铵、甲醇、乙腈、异丙醇、四氢呋喃(THF)(色谱纯);单硬脂酸甘油酯(批号:J22111117,含量:99%)、三硬脂酸甘油酯(批号:F2214266,含量:99%)、单棕榈酸甘油酯(批号:I2207184,含量:≥95%)、三棕榈酸甘油酯(批号:J2228571,含量:98%)(阿拉丁公司);二硬脂酸甘油酯(批号:C14865624,含量:97%,麦克林公司);二棕榈酸甘油酯(批号:1113-RE-0050,含量:98.5%,CATO公司);单双硬脂酸甘油酯样品(来自A~F 6个不同厂家,不同来源的单双甘油酯样品呈现出不同的形态)。

2 方法与结果

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2.1 对照品与供试品溶液的制备

精密称取6种甘油酯对照品各适量,加四氢呋喃溶解并稀释至10 μg·mL^-1,作为硬脂酸甘油酯混合对照品溶液;取A、B、C、D、E、F6个厂家的单双甘油酯样品,加四氢呋喃溶解并稀释至10 μg·mL^-1,作为各厂家的供试品溶液。

2.2 色谱条件^[15]

使用Kinetex C₁₈柱(2.1 mm×100 mm,2.6 μm),流速为0.3 mL·min^-1,进样盘温度:15 ℃,柱温:45 ℃,甲醇-乙腈-水(1∶1∶1,含5 mmol·L^-1乙酸铵)为流动相A,异丙醇(含5 mmol·L^-1乙酸铵)为流动相B,梯度洗脱见表1;进样量:1 μL。

2.3 质谱条件

质谱的数据采集在配备电喷雾电离源的离子阱飞行时间质谱仪上完成的,采用正负离子同时监测总离子流图(TIC)。母离子m/z 200~1 200(累计时间0.15 s),子离子m/z 100~ 1 200(累计时间25 ms)。气帘气压力(CUR)241.3 kPa,雾化气压力(GS1)379.2 kPa,辅助气压力(GS2)379.2 kPa,喷雾电压(ISVF)5 500 V/-4 500 V(+/-),雾化温度(TEM)550 ℃。

2.4 供试品与对照品溶液的测定

精密量取四氢呋喃空白溶剂、甘油酯混合对照品溶液、A~F 6个厂家的供试品溶液各1 μL直接进样,TIC图见图1~8。由于四氢呋喃与流动相存在极性差异,空白溶剂中呈现出多个特征离子峰,扣除空白溶剂峰后,各组分间并无显著干扰,TIC图上可以直观看到各组分的占比高低。

2.5 数据结果分析

参照面积归一化法,归属了6种不同来源单双甘油酯样品中19种脂肪酸甘油酯的组成和比例,为不同来源单双甘油酯质量等同性的内在机制提供了参考。

由表2结果可知,样品中测得的所有甘油酯均为饱和脂肪酸甘油酯,以棕榈酸和硬脂酸的甘油酯为主,混有一定量的珠光脂酸、油酸、芥酸和木焦油酸的甘油酯;其中含量较高的甘油酯是棕榈酸和硬脂酸的混合甘油二酯和甘油三酯;通过不同企业样品含量柱状图比较,发现不同来源的样品中甘油酯组成比例存在显著差异,但可以看到企业B和E样品构成相似,企业C、D和F样品构成相似(图9)。

3 小结

收起

单双甘油酯无紫外吸收,现行《中国药典》2020年版方法采用RID检测器,且只能分离三甘油酯和二甘油酯,无法分离单甘油酯与游离脂肪酸,不能分析不同脂肪酸与甘油成酯的情况,存在测定方法专属性不强、准确度不高的问题。

本研究以单双甘油酯为对象,聚焦其脂肪酸甘油酯组成,建立了LC-TOF-MS联用测定方法,测定了其中19种脂肪酸甘油酯的组成和比例,为不同来源单双甘油酯质量等同性的内在机制研究提供了参考。未来基于LC-TOF-MS的广泛应用,若该分离方法能够形成标准并推广,将有助于制剂企业对单双硬脂酸甘油酯辅料的质量评价和选择,有望助推国产半固体制剂仿制药一致性评价研究。

基金

收起

湖北省药品监督检验研究院中青年科研基金项目资助(2022YN009)

参考文献

收起

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收起

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2025年第60卷第9期

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doi: 10.11669/cpj.2025.09.012

接收时间：2024-11-08
首发时间：2025-11-11
出版时间：2025-05-01

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收稿日期：2024-11-08

基金

湖北省药品监督检验研究院中青年科研基金项目资助(2022YN009)

作者信息

¹ 湖北省药品监督检验研究院, 湖北省药品质量检测与控制工程技术研究中心, 武汉 430075

² 湖北中医药大学, 武汉 430065

³ 湖北省药品监督管理局药品审评检查中心, 武汉 430077

⁴ 上海爱博才思分析仪器贸易有限公司, 上海 200335

通讯作者:

^*胡敏,女,硕士,正高级工程师研究方向:药品刘晨曦,男,硕士,主管药师研究方向:药品质量控制 Tel:(027)87705266

刘晨曦,男,硕士,主管药师研究方向:药品质量控制 Tel:(027)87705266

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2种不同金属材料的力学参数

科 Family	属数 Number of genus	种数 Number of species	占总种数比例 Percentage of total species (%)	属 Genus	种数 Number of species	占总种数比例 Percentage of total species (%)
鹅膏菌科Amanitaceae	2	11	5.26	鹅膏菌属 Amanita	10	4.78
小菇科 Mycenaceae	2	12	5.74	丝盖伞属 Inocybe	5	2.39
多孔菌科 Polyporaceae	8	14	6.70	蜡蘑属 Laccaria	5	2.39
红菇科 Russulaceae	3	23	11.00	小皮伞属 Marasmius	6	2.87
				小菇属 Mycena	11	5.26
				光柄菇属 Pluteus	5	2.39
				红菇属 Russula	17	8.13
				栓菌属 Trametes	5	2.39

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RefWorks
TxT

t/min	B/%
0	20
0.5	20
1.5	40
3	60
13	98
14.5	98
14.6	20
17	20

t/min

B/%

0.5

1.5

14.5

14.6

No.	t_R /min	m/z (Average)	Glyceride	Formula	Adduct type	Mixture of GTS, GTP,GDP, GDS,GMP and GMS	Manufacture
1	2.946	348.311 08	MG 16∶0	C₁₉H₃₈O₄	[M+NH4]⁺	0.12%	0.48%	0.48%	0.55%	0.47%	0.73%	0.37%
2	3.443	376.342 02	MG 18∶0	C₂₁H₄₂O₄	[M+NH4]⁺	0.15%	0.83%	1.02%	0.79%	0.68%	1.16%	0.48%
3	3.880	404.373 05	MG 20∶0	C₂₃H₄₆O₄	[M+NH4]⁺	0.00%	0.03%	0.02%	0.02%	0.02%	0.02%	0.01%
4	5.030	530.477 57	DG 28∶0\|DG 12∶0_16∶0	C₃₁H₆₀O₅	[M+NH4]⁺	0.02%	0.34%	0.04%	0.08%	0.12%	0.03%	0.07%
5	5.477	558.508 58	DG 30∶0\|DG 14∶0_16∶0	C₃₃H₆₄O₅	[M+NH4]⁺	0.24%	0.98%	0.35%	0.57%	0.58%	0.23%	0.55%
6	5.972	586.539 87	DG 32∶0\|DG 16∶0_16∶0	C₃₅H₆₈O₅	[M+NH4]⁺	9.41%	11.98%	10.94%	12.12%	10.33%	15.15%	11.26%
7	6.488	614.571 39	DG 34∶0\|DG 16∶0_18∶0	C₃₇H₇₂O₅	[M+NH4]⁺	14.24%	19.61%	27.20%	19.28%	16.52%	30.48%	17.93%
8	6.752	628.586 85	DG 35∶0\|DG 17∶0_18∶0	C₃₈H₇₄O₅	[M+NH4]⁺	0.05%	0.08%	0.11%	0.06%	0.06%	0.12%	0.06%
9	7.014	642.602 54	DG 36∶0\|DG 18∶0_18∶0	C₃₉H₇₆O₅	[M+NH4]⁺	5.98%	8.73%	18.96%	8.70%	7.46%	15.91%	7.78%
10	7.544	670.633 47	DG 38∶0\|DG 18∶0_20∶0	C₄₁H₈₀O₅	[M+NH4]⁺	0.18%	0.29%	0.65%	0.30%	0.26%	0.42%	0.27%
11	8.062	698.666 18	DG 40∶0\|DG 16∶0_24∶0	C₄₃H₈₄O₅	[M+NH4]⁺	0.06%	0.48%	0.23%	0.14%	0.12%	0.11%	0.12%
12	8.062	698.664 98	DG 40∶0\|DG 18∶0_22∶0	C₄₃H₈₄O₅	[M+NH4]⁺	0.06%	0.83%	0.23%	0.14%	0.12%	0.11%	0.12%
13	9.389	796.738 16	TG 46∶0\|TG 14∶0_16∶0_16∶0	C₄₉H₉₄O₆	[M+NH4]⁺	1.08%	0.03%	1.00%	1.73%	2.19%	-	1.88%
14	9.822	824.769 38	TG 48∶0\|TG 16∶0_16∶0_16∶0	C₅₁H₉₈O₆	[M+NH4]⁺	18.17%	0.34%	5.67%	14.03%	15.64%	7.17%	15.87%
15	10.029	838.785 08	TG 49∶0\|TG 16∶0_16∶0_17∶0	C₅₂H₁₀₀O₆	[M+NH4]⁺	0.22%	0.98%	0.13%	0.18%	0.20%	0.15%	0.16%
16	10.232	852.800 42	TG 50∶0\|TG16∶0_16∶0_18∶0/TG 16∶0_18∶0_16∶0	C₅₃H₁₀₂O₆	[M+NH4]⁺	28.79%	11.98%	14.45%	23.37%	25.60%	14.61%	24.70%
17	10.421	866.815 67	TG 51∶0\|TG 16∶0_17∶0_18∶0	C₅₄H₁₀₄O₆	[M+NH4]⁺	0.17%	19.61%	0.09%	0.15%	0.13%	0.09%	0.13%
18	10.614	880.831 68	TG 52∶0\|TG 16∶0_18∶0_18∶0/TG 18∶0_16∶0_18∶0	C₅₅H₁₀₆O₆	[M+NH4]⁺	17.30%	0.08%	13.77%	14.50%	15.95%	10.74%	14.88%
19	10.971	908.863 1	TG 54∶0\|TG 18∶0_18∶0_18∶0	C₅₇H₁₁₀O₆	[M+NH4]⁺	3.74%	8.73%	4.65%	3.29%	3.55%	2.74%	3.36%

No.

t_R
/min

m/z
(Average)

Glyceride

Formula

Adduct
type

Mixture of GTS,
GTP,GDP,
GDS,GMP
and GMS

Manufacture

2.946

348.311 08

MG 16∶0

C₁₉H₃₈O₄

[M+NH4]⁺

0.12%

0.48%

0.55%

0.47%

0.73%

0.37%

3.443

376.342 02

MG 18∶0

C₂₁H₄₂O₄

[M+NH4]⁺

0.15%

0.83%

1.02%

0.79%

0.68%

1.16%

0.48%

3.880

404.373 05

MG 20∶0

C₂₃H₄₆O₄

[M+NH4]⁺

0.00%

0.03%

0.02%

0.01%

5.030

530.477 57

DG 28∶0|DG 12∶0_16∶0

C₃₁H₆₀O₅

[M+NH4]⁺

0.02%

0.34%

0.04%

0.08%

0.12%

0.03%

0.07%

5.477

558.508 58

DG 30∶0|DG 14∶0_16∶0

C₃₃H₆₄O₅

[M+NH4]⁺

0.24%

0.98%

0.35%

0.57%

0.58%

0.23%

0.55%

5.972

586.539 87

DG 32∶0|DG 16∶0_16∶0

C₃₅H₆₈O₅

[M+NH4]⁺

9.41%

11.98%

10.94%

12.12%

10.33%

15.15%

11.26%

6.488

614.571 39

DG 34∶0|DG 16∶0_18∶0

C₃₇H₇₂O₅

[M+NH4]⁺

14.24%

19.61%

27.20%

19.28%

16.52%

30.48%

17.93%

6.752

628.586 85

DG 35∶0|DG 17∶0_18∶0

C₃₈H₇₄O₅

[M+NH4]⁺

0.05%

0.08%

0.11%

0.06%

0.12%

0.06%

7.014

642.602 54

DG 36∶0|DG 18∶0_18∶0

C₃₉H₇₆O₅

[M+NH4]⁺

5.98%

8.73%

18.96%

8.70%

7.46%

15.91%

7.78%

7.544

670.633 47

DG 38∶0|DG 18∶0_20∶0

C₄₁H₈₀O₅

[M+NH4]⁺

0.18%

0.29%

0.65%

0.30%

0.26%

0.42%

0.27%

8.062

698.666 18

DG 40∶0|DG 16∶0_24∶0

C₄₃H₈₄O₅

[M+NH4]⁺

0.06%

0.48%

0.23%

0.14%

0.12%

0.11%

0.12%

8.062

698.664 98

DG 40∶0|DG 18∶0_22∶0

C₄₃H₈₄O₅

[M+NH4]⁺

0.06%

0.83%

0.23%

0.14%

0.12%

0.11%

0.12%

9.389

796.738 16

TG 46∶0|TG 14∶0_16∶0_16∶0

C₄₉H₉₄O₆

[M+NH4]⁺

1.08%

0.03%

1.00%

1.73%

2.19%

1.88%

9.822

824.769 38

TG 48∶0|TG 16∶0_16∶0_16∶0

C₅₁H₉₈O₆

[M+NH4]⁺

18.17%

0.34%

5.67%

14.03%

15.64%

7.17%

15.87%

10.029

838.785 08

TG 49∶0|TG 16∶0_16∶0_17∶0

C₅₂H₁₀₀O₆

[M+NH4]⁺

0.22%

0.98%

0.13%

0.18%

0.20%

0.15%

0.16%

10.232

852.800 42

TG 50∶0|TG16∶0_16∶0_18∶0/TG 16∶0_18∶0_16∶0

C₅₃H₁₀₂O₆

[M+NH4]⁺

28.79%

11.98%

14.45%

23.37%

25.60%

14.61%

24.70%

10.421

866.815 67

TG 51∶0|TG 16∶0_17∶0_18∶0

C₅₄H₁₀₄O₆

[M+NH4]⁺

0.17%

19.61%

0.09%

0.15%

0.13%

0.09%

0.13%

10.614

880.831 68

TG 52∶0|TG 16∶0_18∶0_18∶0/TG 18∶0_16∶0_18∶0

C₅₅H₁₀₆O₆

[M+NH4]⁺

17.30%

0.08%

13.77%

14.50%

15.95%

10.74%

14.88%

10.971

908.863 1

TG 54∶0|TG 18∶0_18∶0_18∶0

C₅₇H₁₁₀O₆

[M+NH4]⁺

3.74%

8.73%

4.65%

3.29%

3.55%

2.74%

3.36%